Benzenesulfinic acid → 2-(Benzenesulfonyl)-5-methoxyoxolane

HRID 22481

反応式

HRID 22481 の反応式
[CH3:1][O:2][CH:3]1[CH2:7][CH2:6][CH:5](OC)[O:4]1.[C:10]1([S:16]([OH:18])=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[Cl-].[Ca+2].[Cl-]>C(Cl)Cl>[C:10]1([S:16]([CH:5]2[CH2:6][CH2:7][CH:3]([O:2][CH3:1])[O:4]2)(=[O:18])=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 12057Benzenesulfinic acidHCID 790982,5-DimethoxytetrahydrofuranHCID 5284359Calcium Chloride

生成物 1

HCID 199304622-(Benzenesulfonyl)-5-methoxyoxolane収率 55%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2,5-Dimethoxytetrahydrofuran (17.1 ml, 0.13M) was added dropwise to a stirred solution of benzenesulphinic acid (17.0 g, 0.12M) in dry DCM (100 ml) containing a suspension of powdered calcium chloride (1.0 g) at room temperature under argon. After 4 h, the solution was washed with water (2×50 ml), dried over anhydrous sodium sulphate, filtered and evaporated. The product was crystalised (diethyl ether/hexane) to give 2-benzenesulphonyl-5-methoxytetrahydro-furan as a white crystalline solid (15.9 g, 55%).

後処理

  1. additioncontaining
  2. washthe solution was washed with water (2×50 ml)
  3. dry with materialdried over anhydrous sodium sulphate
  4. filtrationfiltered
  5. customevaporated
  6. customThe product was crystalised (diethyl ether/hexane)

出典と根拠

ORDレコード
ord-b6ed6f7d4f744f7289f901854ca27289
出典データセット
uspto-grants-1995_06
特許番号
US05428168

関連ノート

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