Triethylamine → N-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-ylmethyl)-2-nitrobenzenesulfonamide

HRID 68984

반응식

HRID 68984 반응식
C(N(CC)CC)C.[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([CH2:26][NH2:27])[CH:24]=[CH:25][C:11]1=2)[CH3:9].[N+:28]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[S:37](Cl)(=[O:39])=[O:38])([O-:30])=[O:29].C(=O)(O)[O-].[Na+]>ClCCl>[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([CH2:26][NH:27][S:37]([C:32]3[CH:33]=[CH:34][CH:35]=[CH:36][C:31]=3[N+:28]([O-:30])=[O:29])(=[O:38])=[O:39])[CH:24]=[CH:25][C:11]1=2)[CH3:9]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 155402-Nitrobenzenesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 706570611-Ethyl-3,3,5-trimethyl-7-aminomethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

생성물 1

HCID 66961083N-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-ylmethyl)-2-nitrobenzenesulfonamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triethylamine (0.6 ml) was added to a dichloromethane solution (6 ml) of 1-ethyl-3,3,5-trimethyl-7-aminomethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (1.0 g). The mixture was cooled with ice. 2-Nitrobenzenesulphonyl chloride (0.80 g) was added, and the mixture was stirred at room temperature overnight. A saturated sodium bicarbonate solution was added to the reaction mixture, followed by extraction using dichloromethane.

후처리

  1. temperatureThe mixture was cooled with ice
  2. extractionfollowed by extraction

출처 및 근거

ORD 기록
ord-bd02a9f881a849e5a8322c2181f8cf9b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822453B2

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