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[ CAS No. 1403898-64-5 ] {[proInfo.proName]}

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Chemical Structure| 1403898-64-5
Chemical Structure| 1403898-64-5
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Product Details of [ 1403898-64-5 ]

CAS No. :1403898-64-5 MDL No. :MFCD28100885
Formula : C11H22N2O3 Boiling Point : -
Linear Structure Formula :- InChI Key :OCHKRKFPKUAHGF-RKDXNWHRSA-N
M.W : 230.30 Pubchem ID :71003242
Synonyms :

Safety of [ 1403898-64-5 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H302-H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 1403898-64-5 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 1403898-64-5 ]

[ 1403898-64-5 ] Synthesis Path-Downstream   1~10

  • 1
  • [ 1403898-64-5 ]
  • [ 501-53-1 ]
  • [ 1403898-70-3 ]
YieldReaction ConditionsOperation in experiment
87% With sodium hydroxide; In tetrahydrofuran; water; at 0 - 10℃; for 1h;Inert atmosphere; A solution of 180 <strong>[1403898-64-5]tert-butyl (2R,5R)-5-(hydroxymethyl)-2-methylpiperazine-1-carboxylate</strong> (18.5 g, 80.33 mmol) in 78 THF (190 ml) was cooled in an ice-bath to 0 C. Aqueous 1M 38 sodium hydroxide solution (88 ml, 88.36 mmol) was added, followed by 317 benzyl chloroformate (11.99 ml, 84.34 mmol) (internal reaction temperature kept 57 ethyl acetate in 58 heptane. Pure fractions were evaporated to dryness to afford 318 1-benzyl 4-tert-butyl (2R,5R)-2-(hydroxymethyl)-5-methylpiperazine-1,4-dicarboxylate (25.4 g, 87%) as a colourless oil. 1H NMR (400 MHz, CD3OD, 30 C.): 1.12 (3H, dd), 1.46 (9H, s), 3.1-3.29 (2H, m), 3.53-3.66 (2H, m), 3.81 (1H, d), 3.88-4.02 (1H, m), 4.15-4.38 (2H, m), 5.06-5.26 (2H, m), 7.21-7.51 (5H, m). One exchangeable proton not seen. m/z: ES+ [M-Boc]=265.1.
With sodium hydroxide; In tetrahydrofuran; at 3 - 4℃; for 2h; Preparation 10: (2R,5R)-2-Hydroxymethyl-5-methyl-piperazine-1 ,4-dicarboxylic acid 1 - benzyl ester 4-ferf-butyl esterTo (2R,5R)-5-hydroxymethyl-2-methyl-piperazine-1 -carboxylic acid ie f-butyl ester (21 g, 90 mmol) in THF (210 mL) at 3-4 C (ice bath) was added 1 M aqueous NaOH (99.5 mL) and benzyl chloroformate (12.9 mL, 90.43 mmol). After stirring for 1 h at the same temperature, the mixture was left to stir for another 1 h and then warmed to RT. The organic layer was separated and the aqueous phase extracted with EtOAc (2 x 50 mL). The combined organic extracts were washed with saturated brine solution (150 mL), then dried over sodium sulfate, filtered and concentrated. The crude oil was purified by column chromatography on silica gel (gradient elution, 0 - 100%, EtOAc/petrol), to give the title compound (26 g) as a pale yellow oil, used directly in Preparation 1 1 . 1H NMR (Me-d3-OD): 7.47-7.15 (5H, m), 5.26-5.07 (2H, m), 4.25 (2H, s), 4.04-3.88 (1 H, m), 3.83 (1 H, d), 3.61 (2H, bs), 3.31 -3.09 (2H, m), 1 .48 (9H, s), 1.14 (3H, t).
  • 2
  • [ 67-56-1 ]
  • tert-butyl dicarbonate [ No CAS ]
  • [ 142-64-3 ]
  • [ 1403898-64-5 ]
YieldReaction ConditionsOperation in experiment
75% Preparation 5: (2R,5R)-5-Hydroxymethyl-2-methyl-piperazine-1 -carboxylic acid ferf-butyl ester. To the piperazine dihydrochloride (20 g, 1 19 mmol) in MeOH (96 mL) at 0 C (ice bath) was added triethylamine (48.7 mL, 357 mmol). ie f-Butyl dicarbonate (61 g, 280 mmol) in MeOH (145 mL) was added over 30 min. The reaction temperature was maintained at <10 C for 1 h, warmed to ambient temperature over 1 h and then heated to 50 C for 18 h. The reaction was concentrated and the residue dissolved in ethanol (397 mL). A solution of NaOH (23.8 g, 595 mmol) in water (397 mL) was added and the reaction heated to 100 C for 18 h, then cooled to ambient temperature. Mixture was neutralised with 1 M HCI (-300 mL) to pH 9 (using a pH meter), then extracted with chloroform (3 x 700 mL), dried over sodium sulfate, filtered and concentrated. The residue was redissolved in MeOH and concentrated, then dried in vacuo at 40 C, to give the title compound (21 g, 75%) as a colourless solid. 1H NMR (Me-d3- OD): 4.20-4.07 (1 H, m), 3.79 (1 H, dd), 3.71 -3.58 (2H, m), 3.54 (1 H, dd), 3.24 (1 H, dd), 3.18- 3.01 (1 H, m), 3.01 -2.89 (1 H, m), 2.55 (1 H, dd), 1.48 (9H, s), 1.25 (3H, s).
  • 3
  • [ 1403898-64-5 ]
  • [ 1403898-66-7 ]
  • 4
  • [ 1403898-64-5 ]
  • [ 1403898-67-8 ]
  • 5
  • [ 1403898-64-5 ]
  • [ 1403898-69-0 ]
  • 6
  • [ 1403898-64-5 ]
  • (2R,5R)-5-methyl-piperazine-1,2,4-tricarboxylic acid 1-benzyl ester 4-tert-butyl ester [ No CAS ]
  • 7
  • [ 1403898-60-1 ]
  • [ 1403898-64-5 ]
  • [ 1403898-65-6 ]
YieldReaction ConditionsOperation in experiment
75% With tetrahydrofuran; triethylamine; at 65℃; for 3h; Preparation 6: (2R,5R)-4-[2-(6-Chloro-3,3-dimethyl-2,3-dihydro-indol-1 -yl)-2-oxo-ethyl]-5- hydroxymethyl-2-methyl-piperazine-1 -carboxylic acid ferf-butyl esterTo 2-chloro-1 -(6-chloro-3,3-dimethyl-2,3-dihydro-indol-1 -yl)-ethanone (397 mg, 1 .31 mmol) in anhydrous THF (1 .23 mL) was added triethylamine (366 mu, 2.60 mmol) and a solution of (2R,5R)-5-hydroxymethyl-2-methyl-piperazine-1 -carboxylic acid ferf-butyl ester (380 mg, 1 .6 mmol) in anhydrous THF (730 mu). The reaction was heated to 65 C for 3 h, cooled to ambient temperature and the solvent removed in vacuo. The residue was purified by columnchromatography on silica gel (gradient elution, 0-80%, EtOAc/petrol), to give the title compound (447 mg, 75%) as a colourless solid. 1H NMR (Me-d3-OD): 8.15 (1 H, d), 7.20 (1 H, d), 7.09 (1 H, dd), 5.51 (2H, s), 4.23-4.13 (1 H, m), 4.09-3.96 (3H, m), 3.81 -3.65 (2H, m), 3.64-3.47 (2H, m), 2.97-2.82 (2H, m), 2.67 (1 H, dd), 1.48 (9H, s), 1.37 (6H, s), 1 .26-1 .22 (3H, m).
  • 8
  • [ 1403898-62-3 ]
  • [ 1403898-64-5 ]
  • 9
  • [ 24424-99-5 ]
  • ((2R,5R)-5-methyl-piperazin-2-yl)-methanol hydrochloride [ No CAS ]
  • [ 1403898-64-5 ]
YieldReaction ConditionsOperation in experiment
75% With triethylamine; In methanol; at 0 - 50℃; for 20.5h; To ((2R,5R)-5-methyl-piperazin-2-yl)-methanol hydrochloride (20 g, 119 mmol) in MeOH (96 mL) at 0 C (ice bath) was added triethylamine (48.7 mL, 357 mmol). teit-Butyl dicarbonate (61 g, 280 mmol) in MeOH (145 mL) was added over 30 mm. The reaction temperature was maintained at <10 c for 1 h, warmed to ambient temperature over 1 h and then heated to 50 00 for 18 h. The reaction was concentrated and the residue dissolved in ethanol (397 mL). Asolution of NaOH (23.8 g, 595 mmol) in water (397 mL) was added and the reaction heated to 100 00 for 18 h, then cooled to ambient temperature. Mixture was neutralised with 1M HCI (-300 mL) to pH 9 (using a pH meter), then extracted with chloroform (3 x 700 mL), dried over sodium sulfate, filtered and concentrated. The residue was redissolved in MeOH and concentrated, then dried in vacuo at 40 c to give the title compound (21 g, 75%) as acolourless solid. 1H NMR (Me-d3-OD): 4.20-4.07 (1H, m), 3.79 (1H, dd), 3.71-3.58 (2H, m),3.54 (1H, dd), 3.24 (1H, dd), 3.18-3.01 (1H, m), 3.01-2.89 (1H, m), 2.55 (1H, dd), 1.48 (9H,5), 1.25 (3H, 5).
75% Preparation 4: (2R,5R)-5-Hydroxymethyl-2-methyl-pi perazi ne-I -carboxylic acid tert-butyl esterTo ((2R,5R)-5-methyl-piperazin-2-yl)-methanol hydrochloride (20 g, 119 mmol) in MeOH (96mL) at 0 C (ice bath) was added triethylamine (48.7 mL, 357 mmol). teit-Butyl dicarbonate (61g, 280 mmol) in MeOH (145 mL) was added over 30 mm. The reaction temperature wasmaintained at <10 c for 1 h, warmed to ambient temperature over 1 h and then heated to 50 cfor 18 h. The reaction was concentrated and the residue dissolved in ethanol (397 mL). Asolution of NaOH (23.8 g, 595 mmol) in water (397 mL) was added and the reaction heated to100 00 for 18 h, then cooled to ambient temperature. Mixture was neutralised with 1M HCI(-300 mL) to pH 9 (using a pH meter), then extracted with chloroform (3 x 700 mL), dried over sodium sulfate, filtered and concentrated. The residue was redissolved in MeOH andconcentrated, then dried in vacuo at 40 c to give the title compound (21 g, 75%) as acolourless solid. 1H NMR (Me-d3-OD): 4.20-4.07 (1H, m), 3.79 (1H, dd), 3.71-3.58 (2H, m), 3.54 (1H, dd), 3.24 (1H, dd), 3.18-3.01 (1H, m), 3.01-2.89 (1H, m), 2.55 (1H, dd), 1.48 (9H, 5), 1.25 (3H, 5).
75% To ((2 R, 5R)-5-methyl-pi perazin-2-yl)-methanol hydrochloride (which may be prepared asdescribed in Preparation 3) (20 g, 119 mmol) in MeOH (96 mL) at 0C (ice bath) was added triethylamine (48.7 mL, 357 mmol). teit-Butyl dicarbonate (61 g, 280 mmol) in MeOH (145 mL) was added over 30 mm. The reaction temperature was maintained at <10 c for 1 h, warmed to ambient temperature over 1 h and then heated to 50 c for 18 h. The reaction was concentrated and the residue dissolved in ethanol (397 mL). A solution of NaOH (23.8 g, 595 mmol) in water(397 mL) was added and the reaction heated to 100 c for 18 h, then cooled to ambient temperature. Mixture was neutralised with 1 M HCI (-300 mL) to pH 9 (using a pH meter), then extracted with chloroform (3 x 700 mL), dried over sodium sulfate, filtered and concentrated. The residue was redissolved in MeOH and concentrated, then dried in vacuo at 40 C to give the title compound (21 g, 75%) as a colourless solid. 1H NMR (Me-d3-OD): 4.20-4.07 (1H, m),3.79 (1H, dd), 3.71-3.58 (2H, m), 3.54 (1H, dd), 3.24 (1H, dd), 3.18-3.01 (1H, m), 3.01-2.89 (1H, m), 2.55 (1H, dd), 1.48 (9H, 5), 1.25 (3H, 5).
  • 10
  • [ 1403898-64-5 ]
  • 1-[(2R,5R)-1-(2-{6-[(4-fluorophenyl)methyl]-3,3-dimethyl-1H,2H,3H-pyrrolo[3,2-b]pyridin-1-yl}2-oxo-ethyl)-5-methylpiperazin-2-yl]methyl}-1H-imidazole-2-carbonitrile L-lactate [ No CAS ]
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