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CAS No. : | 71432-55-8 | MDL No. : | MFCD06657672 |
Formula : | C11H24N2O | Boiling Point : | - |
Linear Structure Formula : | CO(NHC3H7)2C4H8 | InChI Key : | FESDUDPSRMWIDL-UHFFFAOYSA-N |
M.W : | 200.32 | Pubchem ID : | 11041782 |
Synonyms : |
|
Chemical Name : | tert-Butyl N,N'-diisopropylcarbamimidate |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-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 |
---|---|---|
75% | In dichloromethane; for 52h;Heating / reflux; | Example 8; (2E)-3-{4-[({1-[({3-cycIohexyI-1-[2-(4-methylpiperazin-1-yI)-2- oxoethyl]-2-phenyl-1H-indol-6-yl}carbonyl)amino]cyclopentyl }carbonyl) amino]rhohenyI}acryli acid; Step 1; tert-butyl 3-cycIohexyl-1H-indole-6-carboxylate; A solution of 3-cycIohexenyl-1H -indole-6-carboxylic acid (1 eq., prepared as described in Example 1, Step 1) in dry DCM (0,19 M) was treated with tert-butyl N,N'-diisopropylimidocarbamate (2 eq.). The resulting clear solution was heated at reflux for 36 h. Addition of a further equivalent of isourea was required after 16 h to drive the reaction to completion. After cooling down the solvent was evaporated giving a residue that was purified by silica gel chromatography (Flashmaster Personal, PE: EtOAc, 30:1) affording tert-butyl 3-cyclohexyl-1H-indole-6-carboxylate (75percent) |
58% | In dichloromethane; for 19h;Heating / reflux; | Step 4: tert-butyl S-cvclohexyl-lH-indole--carboxylate; 2 eq of tert-buty\\ N,N-diisopropylimidocarbamate (prepared according to literature precedent: Synthesis1979, 561) were added to a solution of 3-cyclohexyl-l//-indole-6-carboxylic acid (prepared as described in published International patent application WO2004087714) in CH2Cl2 (0.4 M) and the mixture heated at reflux under N2 for 16 h. A further 2.5 eq of tert-butyl N,N-diisopropylimidocarbamate were then added portionwise over 3 h, with heating being resumed after each addition. The reaction mixture was then filtered whilst hot through a pad of celite and the filtrate concentrated in vacuo. The residue was purified by flash chromatography (5percent EtOAc/PE) to afford the title compound (58 percent); MS (ES") m/z 298 (M-H)". |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
7.2 g | In tetrahydrofuran; at 20℃; for 2h;Inert atmosphere; | DIC (12.1 mL, 77.8 mmol) was added to a mixture of CuCl (140 mg, 1.4 mmol) and tert-butanol (29.9 mL, 312.6 mmol) and the mixture was stirred at room temperature for 12 h. The volatile components were removed under reduced pressure. The solid was dissolved in THF (25 mL) and 5-methoxy-2-methyl-1H-indole-3-acetic acid (2) (7.0 g, 31.9 mmol) was added and the mixture stirred at room temperature for 2 h. The solvent was evaporated and the solid was purified by column chromatography with a mixture of hexanes (80-100 C) and ethyl acetate (3:1). The solvent was removed under reduced pressure to yield a white solid. Yield: 7.2 g (82%); elemental Anal. Calcd for C16H21NO3: C, 69.80; H, 7.69. Found: C, 69.57; H, 7.67; mp: 110-111 C; ESI MS (-) (CH3COCH3): m/z: 274.0 (100%, [M-H]-); 1H NMR (CDCl3, ppm): 7.75 (s, vbr, NHindole), 7.14 (d, 3JHH = 8 Hz, 1H, CHindole), 7.00 (d, 4JHH = 2 Hz, 1H, CHindole), 6.76 (dd, 3JHH = 8 Hz, 4JHH = 2 Hz, 1H, CHindole), 3.85 (s, 3H, OCH3), 3.54 (s, 2H, CH2), 2.39 (s, 3H, CH3), 1.43 (s, 9H, C(CH3)3); 13C{1H} NMR (CDCl3, ppm): 171.4 (COO), 154.0 (CindoleO), 133.5 (Cindole), 130.2 (Cindole), 129.1 (Cindole), 110.9 (CindoleH), 110.9 (CindoleH), 105.0 (Cindole), 100.6 (CindoleH), 80.5 (C(CH3)3), 55.9 (OCH3), 31.9 (CH2), 28.1 (C(CH3)3), 11.9 (CH3); IR (selected, KBr, cm-1): = 3342 (s, nu(N-H)), 3005 (w), 2980 (w), 2965 (w), 2914 (w), 2837 (w), 2047 (w), 1722 (s, nu(CO)). |
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