Thionyl Chloride → HCID 178499150、化合物

HRID 535914ノート

反応式

HRID 535914 の反応式
[CH2:1]([N:8]([CH2:12][C:13]1[N:14]=[CH:15][NH:16][C:17]=1[C:18]([O:20][CH3:21])=[O:19])[CH2:9][CH2:10]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:24])=O>C(Cl)Cl>[ClH:24].[CH2:1]([N:8]([CH2:12][C:13]1[N:14]=[CH:15][NH:16][C:17]=1[C:18]([O:20][CH3:21])=[O:19])[CH2:9][CH2:10][Cl:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 178499151HCID 178499151、化合物

生成物 1

HCID 178499150HCID 178499150、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
44 °C

実験手順

To a solution of Intermediate 1D (0.94 g, 3.24 mmol) in DCM (30 mL) was added thionyl chloride (0.95 mL, 12.96 mmol). The resulting mixture was stirred at 44° C. overnight and allowed to cool to ambient temperature. The mixture was concentrated under reduced pressure, azeotroped with acetonitrile and dried under vacuum overnight to give Intermediate 1E in quantitative yield as a white solid which was used in the next step without further purification.

後処理

  1. temperatureto cool to ambient temperature
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customazeotroped with acetonitrile
  4. customdried under vacuum overnight

出典と根拠

ORDレコード
ord-c8d5b72adee54506b4b87124fbffdcb6
出典データセット
uspto-grants-2014_10
特許番号
US08859538B2

反応ノート

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