Trimethylamine → (2-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylamino}-ethyl)-trimethyl-ammonium chloride

HRID 1519478노트

반응식

HRID 1519478 반응식
[CH3:1][N:2]([CH3:4])[CH3:3].[Cl:5][C:6]1[CH:42]=[CH:41][C:9]2[N:10]([C:22](=[O:40])[C:23]3[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[CH3:37])=[CH:25][C:24]=3[CH3:39])[CH2:11][CH2:12][CH2:13][CH:14]([O:15][C:16](=[O:21])[NH:17][CH2:18][CH2:19]Cl)[C:8]=2[CH:7]=1>C(O)C>[Cl-:5].[Cl:5][C:6]1[CH:42]=[CH:41][C:9]2[N:10]([C:22](=[O:40])[C:23]3[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[CH3:37])=[CH:25][C:24]=3[CH3:39])[CH2:11][CH2:12][CH2:13][CH:14]([O:15][C:16]([NH:17][CH2:18][CH2:19][N+:2]([CH3:4])([CH3:3])[CH3:1])=[O:21])[C:8]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 1146TrimethylamineHCID 86708937{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl} (2-chloroethyl)carbamate

생성물 1

HCID 66733336(2-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylamino}-ethyl)-trimethyl-ammonium chloride

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
170 °C

실험 절차

Trimethylamine (30% solution, 0.5 ml) was added to an ethanol solution (10 ml) of {7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl}(2-chloroethy)carbamate (330 mg), and the mixture was heated at 170° C. for 15 minutes (microwave reactor). After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. To the residue was added ethyl acetate, and the resulted precipitates were collected by filtration and dried to obtain 120 mg of (2-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylamino}-ethyl)-trimethyl-ammonium chloride as white powder.

후처리

  1. temperatureAfter cooling to room temperature
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. additionTo the residue was added ethyl acetate
  4. customthe resulted precipitates
  5. filtrationwere collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-67a158e7e0af4212bfc2efd29c842dd4
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073868B2

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