Thionyl Chloride → HCID 178499150, 화합물

HRID 535914노트

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HRID 535914 반응식
[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

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 178499151HCID 178499151, 화합물

생성물 1

HCID 178499150HCID 178499150, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
44 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c8d5b72adee54506b4b87124fbffdcb6
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859538B2

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