4-Toluenesulfonyl chloride → HCID 12735323、化合物

HRID 1614009

反応式

HRID 1614009 の反応式
[OH-:1].[K+].[C:3]1([CH:9]([OH:18])[CH:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[OH:11])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[S:19](Cl)([C:22]1[CH:28]=[CH:27][C:25]([CH3:26])=[CH:24][CH:23]=1)(=[O:21])=[O:20]>CCOCC>[C:25]1([CH3:26])[CH:27]=[CH:28][C:22]([S:19]([O:18][CH:9]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:10]([O:11][S:19]([C:22]2[CH:28]=[CH:27][C:25]([CH3:26])=[CH:24][CH:23]=2)(=[O:20])=[O:1])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:21])=[O:20])=[CH:23][CH:24]=1

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 14797Potassium HydroxideHCID 95447Hydrobenzoin

生成物 1

HCID 12735323HCID 12735323、化合物収率 412.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Potassium hydroxide (400 mg, 7.0 mmole) was added to a solution of 1,2-diphenylethane-l,2-diol (I40 mg, 0.65 mmole) in dry ether (30 mL). TsCl (286 mg, 1.5 mmole) was added. The reaction was completed after 1 hour with stirring under N2 atmosphere at RT. A white solid was obtained. The white solid was filtered and washed with dichloromethane. The combined filtrate was concentrated, Recrystallization with methylene chloride and hexane gave the crystalline solid (1.4 g, 44.6%), mp, 110-112 (decomposed), 'H-NMR(CDCl3) δ, 2.39(s, 6H CH3), 5.61(s, 2H, CH), 6.89-7.55(m, 18H, ArH).

後処理

  1. customA white solid was obtained
  2. filtrationThe white solid was filtered
  3. washwashed with dichloromethane
  4. concentrationThe combined filtrate was concentrated
  5. customRecrystallization with methylene chloride and hexane

出典と根拠

ORDレコード
ord-3c319cfc1762498f9802c93a6ad54e50
出典データセット
uspto-grants-1993_03
特許番号
US05194651

関連ノート

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