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

HRID 363048

反応式

HRID 363048 の反応式
[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

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 70352Benzyl Phenyl Ether

生成物 1

HCID 47383854-(Benzyloxy)benzene-1-sulfonyl chloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c64f0a7157d94fdfb0a6656623c089b3
出典データセット
uspto-grants-1999_02
特許番号
US05872138

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