2-氯-2-苯基苯乙酮 → 2-(3,4-Methylenedioxyphenyl)-4,5-diphenylthiazole

HRID 2049275

反应方程式

HRID 2049275 反应方程式
[C:1]([NH2:12])(=[S:11])[C:2]1[CH:10]=[CH:9][C:8]2[O:7][CH2:6][O:5][C:4]=2[CH:3]=1.[C:13]1([C:19]([CH:21](Cl)[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=O)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(O)C>[CH2:6]1[O:7][C:8]2[CH:9]=[CH:10][C:2]([C:1]3[S:11][C:19]([C:13]4[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=4)=[C:21]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[N:12]=3)=[CH:3][C:4]=2[O:5]1

参与物

4

反应物 2

HCID 953432-氯-2-苯基苯乙酮HCID 27761263,4-(亚甲基二氧基)硫代甲酰氨

产物 1

HCID 203449832-(3,4-Methylenedioxyphenyl)-4,5-diphenylthiazole收率 67.1%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

Thiopiperonylamide (18.1 g, 0.10 mole) and desyl chloride (23.1 g, 0.10 mole) are heated under reflux in 95% ethanol (100 ml) for two hours. An oil precipitates which solidifies when the reaction mixture is cooled. The solid is collected and recrystallized from ethanolethyl acetate to give 24.0 g (67% yield ) of 2-(3,4-methylenedioxyphenyl)-4,5-diphenylthiazole, m.p. 121°-124° C. Thiopiperonylamide is also prepared from the corresponding nitrile by the method of Fairfull et al., J. Chem. Soc. 1952, 742.

后处理

  1. customAn oil precipitates which
  2. temperatureis cooled
  3. customThe solid is collected
  4. customrecrystallized from ethanolethyl acetate

来源与证据

ORD记录
ord-52f6e35e790d48d48e59f5d026142358
来源数据集
uspto-grants-1980_04
专利号
US04197306

关联笔记

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