Dimethylformamide → 7-Chloro-9-(1-chloroethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one

HRID 626825ノート

反応式

HRID 626825 の反応式
N1C(Cl)=NC(Cl)=NC=1[Cl:3].[Cl:10][C:11]1[CH:12]=[C:13]([CH:24](O)[CH3:25])[C:14]2[O:20][CH2:19][CH2:18][NH:17][C:16](=[O:21])[C:15]=2[C:22]=1[CH3:23].CN(C)C=O>C(Cl)Cl>[Cl:10][C:11]1[CH:12]=[C:13]([CH:24]([Cl:3])[CH3:25])[C:14]2[O:20][CH2:19][CH2:18][NH:17][C:16](=[O:21])[C:15]=2[C:22]=1[CH3:23]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 7954Cyanuric chlorideHCID 866975197-Chloro-9-(1-hydroxyethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one

生成物 1

HCID 866975207-Chloro-9-(1-chloroethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one収率 70%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of cyanuric chloride (15 mg, 0.079 mmol), 7-chloro-9-(1-hydroxyethyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (14 mg, 0.053 mmol) and N,N-dimethylformamide (20 μL) in methylene chloride (0.4 mL) was stirred at room temperature overnight. The mixture was diluted with methylene chloride, washed with saturated sodium bicarbonate, water, brine, dried over sodium sulfate, filtered and concentrated to give the desired compound (10 mg, 70%).

後処理

  1. washwashed with saturated sodium bicarbonate, water, brine
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4540b44b21964430bed0a6c1e28e027a
出典データセット
uspto-grants-2016_04
特許番号
US09309251B2

反応ノート

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