Triethylamine → Methanesulfonic acid 4-fluoro-5-iodo-2-methanesulfonyloxymethyl-benzyl ester

HRID 1930950노트

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HRID 1930950 반응식
[F:1][C:2]1[C:3]([I:12])=[CH:4][C:5]([CH2:10][OH:11])=[C:6]([CH2:8][OH:9])[CH:7]=1.C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22]>ClCCl.O>[F:1][C:2]1[C:3]([I:12])=[CH:4][C:5]([CH2:10][O:11][S:21]([CH3:20])(=[O:23])=[O:22])=[C:6]([CH2:8][O:9][S:21]([CH3:20])(=[O:23])=[O:22])[CH:7]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 57753608(5-Fluoro-2-hydroxymethyl-4-iodo-phenyl)-methanol

생성물 1

HCID 57753243Methanesulfonic acid 4-fluoro-5-iodo-2-methanesulfonyloxymethyl-benzyl ester수율 67%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a suspension of 8.86 mmol (5-fluoro-2-hydroxymethyl-4-iodo-phenyl)-methanol in 30 ml dichloromethane at 0° C. were added dropwise 22.2 mmol triethylamine and 19.5 mmol methanesulfonyl chloride. The mixture was stirred at 0° C. for 1 h, and then at room temperature for 5 h. The reaction mixture was diluted with water and extracted four times with dichloromethane. The combined organic phases were dried over sodium sulfate and concentrated in vacuo to afford the title compound as a yellow oil (67% yield) which was used in the next step without further purification.

후처리

  1. waitat room temperature for 5 h
  2. extractionextracted four times with dichloromethane
  3. dry with materialThe combined organic phases were dried over sodium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-448434f4ff2b44daa9fb636c947f3672
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188139B2

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