Benzenesulfonyl chloride → Benzenesulfonic acid 3-hydroxy-5-methylphenyl ester

HRID 482250

反応式

HRID 482250 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([CH:8]=1)[OH:7].C(=O)([O-])O.[Na+].[C:15]1([S:21](Cl)(=[O:23])=[O:22])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>CCOCC>[OH:7][C:6]1[CH:5]=[C:4]([O:9][S:21]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)(=[O:23])=[O:22])[CH:3]=[C:2]([CH3:1])[CH:8]=1

参加物

5

反応物 3

HCID 7369Benzenesulfonyl chlorideHCID 10436OrcinolHCID 516892Sodium Bicarbonate

生成物 1

HCID 11054545Benzenesulfonic acid 3-hydroxy-5-methylphenyl ester収率 98.4%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

24.8 g (200 mmol) 5-methyl-resorcinol, 200 ml ether, 400 ml sodium hydrogen carbonate solution and 28.2 ml (220 mmol) benzenesulfonyl chloride were stirred for 2 d at room temperature, the organic phase was separated, the aqueous phase was extracted with ether, the combined organic phases were dried over sodium sulfate, filtered, the solvent was removed in a vacuum and 52 g (quant.) benzenesulfonic acid-3-hydroxy-5-methyl-phenyl ester was obtained. Fp 108°-110° C.

後処理

  1. customthe organic phase was separated
  2. extractionthe aqueous phase was extracted with ether
  3. dry with materialthe combined organic phases were dried over sodium sulfate
  4. filtrationfiltered
  5. customthe solvent was removed in a vacuum

出典と根拠

ORDレコード
ord-4af34506f488478795731140f6f2a309
出典データセット
uspto-grants-1998_08
特許番号
US05795892

関連ノート

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