Chlorosulfonic acid → 2-Fluoro-5-(2-oxo-propyl)-benzenesulfonyl chloride

HRID 2247337노트

반응식

HRID 2247337 반응식
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][C:14](=[O:16])[CH3:15])=[CH:9][CH:8]=1>>[F:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:13][C:14](=[O:16])[CH3:15])=[CH:11][C:12]=1[S:2]([Cl:1])(=[O:5])=[O:3]

참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 521187(4-Fluorophenyl)acetone

생성물 1

HCID 858617322-Fluoro-5-(2-oxo-propyl)-benzenesulfonyl chloride

실험 절차

To chlorosulfonic acid (25 ml, excess) cooled at −10° C. is added dropwise 4-fluorophenyl acetone (1.0 g, 6.57 mmol). The temperature is kept below 0° C. throughout the addition. The reaction mixture is then left to warm up to room temperature overnight. The reaction mixture is poured carefully onto ice (1500 ml). Once ice is melted, the aqueous layer is extracted with DCM (3×250 ml). The combined organic layers are dried over MgSO4, filtered and concentrated to afford the titled compound as an off-white solid.

후처리

  1. additionThe temperature is kept below 0° C. throughout the addition
  2. waitThe reaction mixture is then left
  3. additionThe reaction mixture is poured carefully onto ice (1500 ml)
  4. extractionthe aqueous layer is extracted with DCM (3×250 ml)
  5. dry with materialThe combined organic layers are dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-061bf1faca97485782ebb035a481610c
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07687637B2

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