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 1626042ノート

反応式

HRID 1626042 の反応式
[CH3:1][N:2]([CH3:4])[CH3:3].[Cl:5][CH2:6][CH2:7][NH:8][C:9](=[O:42])[O:10][CH:11]1[CH2:17][CH2:16][CH2:15][N:14]([C:18](=[O:36])[C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:34])[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[CH3:33])=[CH:21][C:20]=2[CH3:35])[C:13]2[CH:37]=[CH:38][C:39]([Cl:41])=[CH:40][C:12]1=2>C(O)C>[Cl-:5].[Cl:41][C:39]1[CH:38]=[CH:37][C:13]2[N:14]([C:18](=[O:36])[C:19]3[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:34])[C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[CH3:33])=[CH:21][C:20]=3[CH3:35])[CH2:15][CH2:16][CH2:17][CH:11]([O:10][C:9]([NH:8][CH2:7][CH2:6][N+:2]([CH3:4])([CH3:3])[CH3:1])=[O:42])[C:12]=2[CH:40]=1

参加物

4

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
170 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f1a664c23a934ddcbd07fafcbfcb65e0
出典データセット
uspto-grants-2014_07
特許番号
US08785386B2

反応ノート

読み込み中…