Добрый день!
Посмотрите,пожалуйста,получение
Cc1n[nH]c(C)c1CCC#N
CC(C)(C)OC(=O)Nc1ccc2NC(=O)C(=O)c2c1
Спасибо!
Поиск в Reaxys
Re: Поиск в Reaxys
есть
(2,3‑dioxo‑2,3‑dihydro‑1H‑indol‑5‑yl)‑carbamic acid tert‑butyl ester
из
5‑Nitroisatin
и
Di‑tert‑butyl iminodicarboxylate
Stage #1: 5-nitroisatin; iminodicarboxylic acid di-tert-butyl ester With hydrogen; 5%-palladium/activated carbon In methanol at 20℃; for 6h;
Stage #2: With dmap In methanol for 5h;
Experimental Procedure
28%
Current Patent Assignee: SUGEN - WO2005/5378, 2005, A2
Location in patent: Page/Page column 75
Experimental Procedure
(2 3-Dioxo-2, 3-DIHYDRO- ? H-INDOL-5-YL1-CARBAMIC ACID TERT-BUTYL ESTER [0360] 5-NITRO-1 H-INDOLE-2, 3-dione (500 mg, 2.60 mmol) was dissolved in methanol (8 ML). Pd/C (5%) (333 mg, 0.16 mmol) was added under nitrogen. The round bottom flask was charged with hydrogen (BALLOON). DI-T-BUTYLDICARBAMATE (840 mg, 3.90 mmol) was added. It was stirred for 6 h at room temperature. 4- (DIMETHYLAMINO) pyridine (16 mg, 0.13 mmol) was added and it was stirred for another 5h. The reaction mixture was filtered through a pad of cellite, the solvent was removed and the residue was purified by silica gel chromatography ethyl acetate/hexane = 3/2). The title compound was obtained as a yellow solid (191 mg, 28%). [0361J H-NMR (400 MHz, D6-DMSO) o 1. 47 (s, 9H), 6. 83 (D, J = 8. 6 Hz, 1H), 7.58 (DD, J = 2.0, 8.2 Hz, 1 H), 7.61 (s, 1 H), 9.42 (S, 1 H), 10.89 (s, 1 H) ; MS m/z (relative intensity, %) 263.3 ([M+1]+, 100).
(2,3‑dioxo‑2,3‑dihydro‑1H‑indol‑5‑yl)‑carbamic acid tert‑butyl ester
из
5‑Nitroisatin
и
Di‑tert‑butyl iminodicarboxylate
Stage #1: 5-nitroisatin; iminodicarboxylic acid di-tert-butyl ester With hydrogen; 5%-palladium/activated carbon In methanol at 20℃; for 6h;
Stage #2: With dmap In methanol for 5h;
Experimental Procedure
28%
Current Patent Assignee: SUGEN - WO2005/5378, 2005, A2
Location in patent: Page/Page column 75
Experimental Procedure
(2 3-Dioxo-2, 3-DIHYDRO- ? H-INDOL-5-YL1-CARBAMIC ACID TERT-BUTYL ESTER [0360] 5-NITRO-1 H-INDOLE-2, 3-dione (500 mg, 2.60 mmol) was dissolved in methanol (8 ML). Pd/C (5%) (333 mg, 0.16 mmol) was added under nitrogen. The round bottom flask was charged with hydrogen (BALLOON). DI-T-BUTYLDICARBAMATE (840 mg, 3.90 mmol) was added. It was stirred for 6 h at room temperature. 4- (DIMETHYLAMINO) pyridine (16 mg, 0.13 mmol) was added and it was stirred for another 5h. The reaction mixture was filtered through a pad of cellite, the solvent was removed and the residue was purified by silica gel chromatography ethyl acetate/hexane = 3/2). The title compound was obtained as a yellow solid (191 mg, 28%). [0361J H-NMR (400 MHz, D6-DMSO) o 1. 47 (s, 9H), 6. 83 (D, J = 8. 6 Hz, 1H), 7.58 (DD, J = 2.0, 8.2 Hz, 1 H), 7.61 (s, 1 H), 9.42 (S, 1 H), 10.89 (s, 1 H) ; MS m/z (relative intensity, %) 263.3 ([M+1]+, 100).