Thionyl Chloride → 4-(N,N-diethylcarbamoyl)benzhydryl chloride

HRID 929652

반응식

HRID 929652 반응식
[CH2:1]([N:3]([CH2:20][CH3:21])[C:4]([C:6]1[CH:19]=[CH:18][C:9]([CH:10](O)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:8][CH:7]=1)=[O:5])[CH3:2].S(Cl)([Cl:24])=O>ClCCl>[CH2:1]([N:3]([CH2:20][CH3:21])[C:4]([C:6]1[CH:19]=[CH:18][C:9]([CH:10]([Cl:24])[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:8][CH:7]=1)=[O:5])[CH3:2]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 105409664-(N,N-diethylcarbamoyl)benzhydryl alcohol

생성물 1

HCID 107330954-(N,N-diethylcarbamoyl)benzhydryl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The 4-(N,N-diethylcarbamoyl)benzhydryl alcohol (61.35 g, 216.5 mmol) was dissolved in 1500 mL of dichloromethane and 23.69 mL (324.8 mmol) of thionyl chloride was added dropwise. The reaction solution was stirred overnight at room temperature and the solvent was removed under vacuum. The crude product was redissolved in 800 mL of toluene and the solvent again was removed under vacuum to eliminate excess thionyl chloride, providing crude 4-(N,N-diethylcarbamoyl)benzhydryl chloride as a dark oil. Crude yield=100%.

후처리

  1. customthe solvent was removed under vacuum
  2. dissolutionThe crude product was redissolved in 800 mL of toluene
  3. customthe solvent again was removed under vacuum

출처 및 근거

ORD 기록
ord-401efd2cf8fd4a3e9b6248fbbcc7eb6f
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296707B2

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