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CAS No. : | 5407-04-5 | MDL No. : | MFCD00012521 |
Formula : | C5H13Cl2N | Boiling Point : | - |
Linear Structure Formula : | (CH3)2NCH2CH2CH2Cl·HCl | InChI Key : | LJQNMDZRCXJETK-UHFFFAOYSA-N |
M.W : | 158.07 | Pubchem ID : | 94308 |
Synonyms : |
3-Chloro-N,N-dimethylpropan-1-amine hydrochloride
|
Chemical Name : | 3-Chloro-N,N-dimethylpropan-1-amine hydrochloride |
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: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
86% | With potassium carbonate; sodium iodide; In acetone;Reflux; | The mixture of 6-hydroxy-2-cyanobenzothiozole(0.311 g, 1.77 mmol), 3-chloropropyldimethylamine hydrochloride (0.36 g, 2.27 mmol), potassium carbonate (0.63g, 4.57 mmol) and sodium iodide (0.034 g) in acetone (30 ml) was heated to reflux overnight. Upon cooling to roomtemperature, the insoluble solid was removed by filtration. The compound was purified by flash chromatography usingmethylene chloride/methanol (96:4) as eluent in a yield of 86percent (0.387 g).1H NMR (CD2Cl2): 7.98 (d, J= 9.3 Hz, 1H), 7.32 (d, J= 2.4 Hz, 1H), 7.16 (dd, J = 9.0 Hz, J= 2.1 Hz, 1H), 4.04 (t, J = 6.4Hz, 2H, OCH2), 2.36 (t, J = 7.2 Hz, 2H, NCH2), 2.13 (s, 6H, CH3), 1.90 (m, 2H, CH2). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With caesium carbonate; In DMF (N,N-dimethyl-formamide); at 60℃; for 28h; | Compound 1 B (2.50 g, 12.3 mm) was dissolved in dry DMF (50 mL) followed by the addition of 3-dimethylaminopropyl chloride hydrochloride (2.34 g, 14.8 mm) and cesium carbonate (10.00 g, 30.7 mm). The mixture was stirred at 60 C for 24 hrs. Additional 3-dimethylaminopropyl chloride hydrochloride (0.5848 g, 3.7 mm) was added and the reaction was stirred at 60 C C for 4 hrs. The mixture was filtered and the filtrate was diluted with ethyl acetate, washed with water (4x) and brine (1X), then dried (NA2SO4) and evaporated in vacuo. The crude product was chromatographed (silica gel 97% DCM/3% MeOH to 95% DCM/5% MeOH) to afford Compound 4c (1.35 G). HNMR (DMSO) 6 1.88- 2.00 (m, 2H, CH2), 2.12 (s, 8H, CH2 and CH3), 3.89 (s, 2H, CH3), 4.34 (t, 2H, CH2), 7.29-7. 38 (m, 2H, H-5 and H-6), 7.67 (d, 1H, H-7), 8.17 (d, 1H, H-4) and 8.49 (s, 1 H, H-2). ES-MS M/Z 289 (MH). Compound 4b (0.060 g, 0.26 mm) and Compound 4c (0.1124 g, 0.39 mm) were dissolved in dry THF (1 mL) followed by the addition of 60% NaH (0.104 g, 2.6 mm). The mixture was stirred at ambient temperature for 3 hrs and then the reaction was quenched with water and extracted with ethyl acetate. The organic layer was washed with water (1X15 mL) and brine (1x15 mL), then dried (NA2SO4), and evaporated in vacuo. The crude product was chromatographed (silica gel-97% DCM/ 1% MeOH/2% NH40H) to afford Compound 31 (0.0275 g, 23%). HNMR (CD30D) 8 0.3793-0. 4566 (m, 2H, CH2), 0. 6618 (s, 6H, CH3), 0.759 (t, 2H, CH2), 2.71 (t, 2H, CH2), 4.85-4. 99 (m, 2H, aromatics), 5.42-5. 61 (m, 3H, aromatics), 5.80 (d, 2H, aromatics), 6.19 (d, 1H, aromatics), 6.38 (d, 2H, aromatics). ES-MS M/Z 464 (MH+). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With NaH; In N,N-dimethyl-formamide; | EXAMPLE 19 3-[1-[3-(dimethylamino)propyl]-1H-indol-3-yl]-4-[1-(3-pyridinyl)-1H-indazol-3-yl]-1H-pyrrole-2,5-dione (Compound 59) The indol-3-yl-glyoxylic methyl ester (0.50 g, 2.46 mmol) Compound 2b and 3-dimethylamino propyl chloride hydrochloride (0.44 g, 2.78 mmol) were combined in DMF (5 mL) and cooled to 0 C. as 95% NaH (135 mg, 5.34 mmol) was added. The reaction vessel was placed in an oilbath at 55 C. for 20 h and then cooled to ambient temperature. The solution was diluted with DCM (30 mL), washed with water, 3 times with saturated NaHCO3 and once with brine, then dried (K2CO3) and evaporated in vacuo to give an oil (0.44 g, 62%). The oil was purified via flash column (DCM:MeOH; 10:1) to afford Compound 19a. ES-MS m/z 289 (MH+). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
25% | With potassium carbonate; In N,N-dimethyl-formamide; at 100 - 110℃; for 24h; | To a solution of <strong>[2737-22-6]2,4,6-tribromo-3-hydroxybenzaldehyde</strong> 15 2a (100 mg, 0.279 mmol) in DMF (1 mL) was added K2CO3 (115 mg, 0.837 mmol) and 2-Chloro-N,N-dimethylpropylamine hydrochloride 3a (62 mg, 0.390 mmol) and the reaction mixture was heated to 100-110 C for 24 h. After completion of the reaction, water (3 mL) was added and the reaction mixture was extracted with EtOAc (8 * 3 mL). Combined organic phases were washed with water (2 mL), brine (2 mL), dried over sodium sulfate, and concentrated in vacuo. The resulting crude was purified over silica gel column chromatography with 15% EtOAc in hexane, which afforded product as colourless solid (24 mg, 25%); mp: 96-98 C; Rf = 0.5 (25% EtOAc in hexane); 1H NMR (400 MHz, CDCl3) δ = 10.14 (s, 1H), 6.84 (s, 1H), 4.26 (t, J = 6.4 Hz, 2H), 3.57 (t, J = 5.4 Hz, 2H), 3.01 (s, 3H), 2.14 (quin, J = 6.3 Hz, 2H); 13C NMR (100 MHz, CDCl3) δ = 190.4, 148.7, 144.5, 121.6, 121.4, 121.3, 119.2, 69.8, 52.2, 41.2, 27.9; IR (neat) = 2928, 2876, 1682, 1565, 1509, 1318, 1274, 1191, 1014, 909; HRMS (ESI+) m/z calculated for C11H12Br2NO2: 347.9235[M+H]+, found: 347.9224. |
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