RMA03230对照品 → 2,4-Dioxo-6-phenylthio-3-oxabicyclo[3.2.0]heptane

HRID 5976

反应方程式

HRID 5976 反应方程式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH:3]=[CH:2]1.[CH:8]([S:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[CH2:9].[Cl-].[Cl-].C([Al+2])C>ClCCCl.C(Cl)Cl>[O:5]=[C:4]1[O:6][C:1](=[O:7])[CH:2]2[CH:3]1[CH2:9][CH:8]2[S:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参与物

6

反应物 3

HCID 7923RMA03230对照品HCID 74572苯基乙烯基硫醚HCID 16686341二氯乙基铝

产物 1

HCID 197942712,4-Dioxo-6-phenylthio-3-oxabicyclo[3.2.0]heptane收率 90.7%

试剂、催化剂与溶剂 2

HCID 111,2-二氯乙烷溶剂HCID 6344二氯甲烷溶剂

实验过程

To a solution of maleic anhydride (0.39 g, 4 mmol) and phenyl vinyl sulfide (0.52, 4 mmol) in 17 mL of 1,2-dichloroethane under nitrogen, was added 2 mL (0.5 equiv) of ethylaluminum dichloride. The resultant solution was stirred at ambient temperature for 0.5 h and then diluted with 75 mL of methylene chloride. The methylene chloride solution was washed three times with saturated aqueous ammonium chloride solution and once with brine, dried over anhydrous sodium sulfate and concentrated to give 0.85 g of the title compound; EI-MS, m/e (rel intensity): 234 (M+, 23), 136 (100), 109 (12), 91 (21).

后处理

  1. washThe methylene chloride solution was washed three times with saturated aqueous ammonium chloride solution
  2. dry with materialonce with brine, dried over anhydrous sodium sulfate
  3. concentrationconcentrated

来源与证据

ORD记录
ord-48761c7d7d1e44d5995d8941f05c8bb3
来源数据集
uspto-grants-1993_09
专利号
US05246931

关联笔记

加载中…