Thionyl Chloride → 1-Allyloxy-3-fluoro-4-chloromethyl-benzene

HRID 2113890노트

반응식

HRID 2113890 반응식
[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11]O)=[C:7]([F:13])[CH:6]=1)[CH:2]=[CH2:3].S(Cl)([Cl:16])=O>ClCCl.CN(C=O)C>[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][Cl:16])=[C:7]([F:13])[CH:6]=1)[CH:2]=[CH2:3]

참가 물질

5

반응물 2

HCID 24386Thionyl ChlorideHCID 69292836(4-Allyloxy-2-fluoro-phenyl)-methanol

생성물 1

HCID 692933781-Allyloxy-3-fluoro-4-chloromethyl-benzene수율 97%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

A solution of 4.20 g (23.1 mmol) (4-allyloxy-2-fluoro-phenyl)-methanol in 80 ml dichloro-methane and 0.5 ml DMF was cooled to 0° C. 2.17 ml (3.57 g, 30.0 mmol) thionyl chloride were added slowly and then stirred for 1 h at room temperature. Dichloromethane was distilled off. The residue was taken up in 100 ml ethyl acetate and washed with concentrated sodium carbonate solution. The organic phase was dried and evaporated to give 4.47 g (97%) 1-allyloxy-3-fluoro-4-chloromethyl-benzene as colored oil.

후처리

  1. distillationDichloromethane was distilled off
  2. washwashed with concentrated sodium carbonate solution
  3. customThe organic phase was dried
  4. customevaporated

출처 및 근거

ORD 기록
ord-3e1914b6e5b347aab30dda1f8f095043
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07432291B2

반응 노트

불러오는 중…