O-[(5-chlorothiophen-2-yl)methyl]hydroxylamine → HCID 53817257，化合物

HRID 1761802笔记

反应方程式

HRID 1761802 反应方程式
[Cl:1][C:2]1[S:6][C:5]([CH2:7][O:8][NH2:9])=[CH:4][CH:3]=1.[C:10]([C:13]1[C:14](=[O:29])[CH2:15][CH:16]([CH:23]2[CH2:28][CH2:27][CH2:26][S:25][CH2:24]2)[CH2:17][C:18]=1[O:19][C:20](=[O:22])[CH3:21])(=O)[CH3:11]>C(O)C>[C:20]([O:19][C:18]1[CH2:17][CH:16]([CH:23]2[CH2:28][CH2:27][CH2:26][S:25][CH2:24]2)[CH2:15][C:14](=[O:29])[C:13]=1[C:10](=[N:9][O:8][CH2:7][C:5]1[S:6][C:2]([Cl:1])=[CH:3][CH:4]=1)[CH3:11])(=[O:22])[CH3:21]

参与物

4

反应物 2

HCID 10986580O-[(5-chlorothiophen-2-yl)methyl]hydroxylamineHCID 20043437HCID 20043437，化合物

产物 1

HCID 53817257HCID 53817257，化合物

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

0.34 g (2.0 mmol) of (5-chlorothien-2-yl)methoxyamine is added to a stirred solution of 0.59 g (2.0 mmol) of 2-acetyl-3-acetyloxy-5-(tetrahydro-2H-thiopyran-3-yl)cyclohex-2-en-1-one in 10 ml of absolute ethanol. After stirring overnight at room temperature, the reaction mixture is concentrated under reduced pressure. The resulting residue is diluted with 25 ml of dichloromethane and washed twice with 10 ml of saturated sodium chloride solution. The washed extract is then dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The product can then be purified by column chromatography employing tetrahydrofuran-hexane (1:2 by volume) as eluent to afford the title compound.

后处理

  1. concentrationthe reaction mixture is concentrated under reduced pressure
  2. additionThe resulting residue is diluted with 25 ml of dichloromethane
  3. washwashed twice with 10 ml of saturated sodium chloride solution
  4. extractionThe washed extract
  5. dry with materialis then dried over anhydrous magnesium sulfate
  6. customevaporated under reduced pressure
  7. customThe product can then be purified by column chromatography

来源与证据

ORD记录
ord-d695c61ca3364c839606a59da6e2bea9
来源数据集
uspto-grants-1989_05
专利号
US04828601

反应笔记

加载中…