Sulfuryl chloride → 4-(Benzyloxy)benzene-1-sulfonyl chloride

HRID 363048

반응식

HRID 363048 반응식
[S:1]([Cl:5])(Cl)(=[O:3])=[O:2].[C:6]1([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>CN(C=O)C>[CH2:13]([O:12][C:6]1[CH:11]=[CH:10][C:9]([S:1]([Cl:5])(=[O:3])=[O:2])=[CH:8][CH:7]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

4

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온도
100 °C

실험 절차

To a 0° C. solution of sulfonyl chloride (1.9 mL, 23.8 mmol) in 2 mL of DMF was added 4.0 g (21.7 mmol) of benzyl phenyl ether (24-1). The resulting solution was then heated at 100° C. for 2 h. The reaction mixture was then cooled and poured onto crushed ice. The aqueous layer was extracted with CH2Cl2 (x3). The combined organic extracts were dried (Na2SO4) and concentrated. Column chromatography (95:5 Hexane/EtOAc) and trituration (hexane) of the pure fractions afforded 24-2 as a pink solid.

후처리

  1. temperatureThe reaction mixture was then cooled
  2. additionpoured
  3. customonto crushed ice
  4. extractionThe aqueous layer was extracted with CH2Cl2 (x3)
  5. dry with materialThe combined organic extracts were dried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c64f0a7157d94fdfb0a6656623c089b3
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05872138

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