氢氧化钾 → 2-氯-3,5-二甲氧苯胺

HRID 58176

反应方程式

HRID 58176 反应方程式
[OH-].[K+].[Cl:3][C:4]1[C:9]([O:10][CH3:11])=[CH:8][C:7]([O:12][CH3:13])=[CH:6][C:5]=1[NH:14]C(=O)C>CCO.O>[Cl:3][C:4]1[C:9]([O:10][CH3:11])=[CH:8][C:7]([O:12][CH3:13])=[CH:6][C:5]=1[NH2:14]

参与物

5

反应物 2

HCID 14797氢氧化钾HCID 56594868N-(2-chloro-3,5-dimethoxyphenyl)acetamide

产物 1

HCID 227430742-氯-3,5-二甲氧苯胺收率 82%

试剂、催化剂与溶剂 2

HCID 702乙醇溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

Potassium hydroxide (2.19 g, 39.18 mmol) was added to a solution of N-(2-chloro-3,5-dimethoxyphenyl)acetamide (1.8 g, 7.837 mmol) in EtOH (100 mL) and water (10 mL) and the reaction mixture heated to reflux for 12 h. Excess EtOH was removed under reduced pressure to obtain a residue. The residue was then partitioned between water and diethyl ether. The organic layer was separated, dried over sodium sulfate, filtered and concentrated under vacuum to afford the title compound (1.2 g, 82% of yield) as a white solid. 1HNMR (CDCl3, 300 MHz): δ 5.97 (s, 2H), 4.08 (brs, 2H), 3.84 (s, 3H), 3.75 (s, 3H); MS (ESI): 188.1 [M+H]+.

后处理

  1. temperaturethe reaction mixture heated
  2. temperatureto reflux for 12 h
  3. customExcess EtOH was removed under reduced pressure
  4. customto obtain a residue
  5. customThe residue was then partitioned between water and diethyl ether
  6. customThe organic layer was separated
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum

来源与证据

ORD记录
ord-e54c098ae5e44c79abbbc706661fc090
来源数据集
uspto-grants-2016_09
专利号
US09434697B2

关联笔记

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