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Water → N-[2-(Chloroacetyl)-5-fluorophenyl]-N-methylformamide

HRID 358664
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HRID 358664 반응식
S(Cl)([Cl:4])(=O)=O.[C:6]([C:9]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:10]=1[N:11]([CH3:14])[CH:12]=[O:13])(=[O:8])[CH3:7].O>ClCCl>[Cl:4][CH2:7][C:6]([C:9]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:10]=1[N:11]([CH3:14])[CH:12]=[O:13])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24648Sulfuryl chlorideHCID 231281532'-acetyl-5'-fluoro-N-methylformanilide

생성물 1

HCID 23128132N-[2-(Chloroacetyl)-5-fluorophenyl]-N-methylformamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of sulphuryl chloride (20.6 ml) in dichloromethane (30 ml) was added dropwise over a period of 45 minutes to the solution of 2'-acetyl-5'-fluoro-N-methylformanilide whilst maintaining the temperature below 2° with ice/water cooling under a nitrogen atmosphere. The mixture was stirred for 3 hours maintaining the temperature below 2°. Water (80 ml) was added dropwise over 15 minutes maintaining the temperature below 10°. The dichloromethane layer was separated and dried over magnesium sulphate to give a solution of 2'-(2-chloroacetyl)-5'-fluoro-N-methylformanilide.

후처리

  1. temperaturemaintaining the temperature below 2°
  2. temperaturemaintaining the temperature below 10°
  3. customThe dichloromethane layer was separated
  4. dry with materialdried over magnesium sulphate

출처 및 근거

ORD 기록
ord-4dcfe2d08b144f06908700d2cfb0a940
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04997840

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