O-[(5-chlorothiophen-2-yl)methyl]hydroxylamine → HCID 136127206，化合物

HRID 1761803笔记

反应方程式

HRID 1761803 反应方程式
[C:1]([C:4]1[C:5](=[O:17])[CH2:6][CH:7]([CH:11]2[CH2:16][CH2:15][CH2:14][S:13][CH2:12]2)[CH2:8][C:9]=1[OH:10])(=O)[CH3:2].[Cl:18][C:19]1[S:23][C:22]([CH2:24][O:25][NH2:26])=[CH:21][CH:20]=1>C(O)C>[Cl:18][C:19]1[S:23][C:22]([CH2:24][O:25][N:26]=[C:1]([C:4]2[C:5](=[O:17])[CH2:6][CH:7]([CH:11]3[CH2:16][CH2:15][CH2:14][S:13][CH2:12]3)[CH2:8][C:9]=2[OH:10])[CH3:2])=[CH:21][CH:20]=1

参与物

4

反应物 2

HCID 10986580O-[(5-chlorothiophen-2-yl)methyl]hydroxylamineHCID 15614621HCID 15614621，化合物

产物 1

HCID 136127206HCID 136127206，化合物收率 95%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂2 次

实验过程

A solution containing 5.1 g (0.020 mol) of 2-acetyl-3-hydroxy-5-(tetrahydro-2H-thiopyran-3-yl)cyclohex-2-en-1-one and 3.4 g (0.021 mol) of (5-chlorothien-2-yl)methoxyamine in 200 ml of ethanol was stirred overnight (about 14 hours) at room temprature and then evaporated to remove ethanol. The concentrate was diluted with 150 ml of methylene chloride and then washed with 100 ml of water and then with 100 ml of saturated aqueous sodium chloride solution. The washed methylene chloride solution was dried over anhydrous magnesium sulfate and then evaporated to dryness under reduced pressure to afford a white solid. Recrystallation of this solid absolute ethanol afforded 7.6 g of the title compound, m.p. 154°-155° C.

后处理

  1. customevaporated
  2. customto remove ethanol
  3. additionThe concentrate was diluted with 150 ml of methylene chloride
  4. washwashed with 100 ml of water
  5. dry with materialThe washed methylene chloride solution was dried over anhydrous magnesium sulfate
  6. customevaporated to dryness under reduced pressure
  7. customto afford a white solid

来源与证据

ORD记录
ord-2ce1995f75d54ea3840fee27d589ec9f
来源数据集
uspto-grants-1989_05
专利号
US04828601

反应笔记

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