二甲基对苯二胺二盐酸 → 3-甲氧基-4-氯苯胺

HRID 29508

反应方程式

HRID 29508 反应方程式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[CH:4][C:3]=1[O:11][CH3:12].[OH-].[Na+]>CO.Cl>[CH3:12][O:11][C:3]1[CH:4]=[C:5]([CH:6]=[CH:7][C:2]=1[Cl:1])[NH2:8]

参与物

5

反应物 2

HCID 14798二甲基对苯二胺二盐酸HCID 705192-氯-5-硝基茴香醚

产物 1

HCID 131036923-甲氧基-4-氯苯胺

试剂、催化剂与溶剂 2

HCID 313海萝胶溶剂HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

反应条件

温度
50 °C

实验过程

2-Chloro-5-nitro anisole (6.0 g, 0.032 mol) in MeOH (45 ml) was added slowly to stannous chloride (15.1 g, 0.08 mol) in conc. HCl (110 ml) at 40° C. and the temperature was slowly raised to 50° C. Stirring was continued for 2 h. After cooling to RT, the reaction mixture was basified with 50% NaOH solution, extracted by ethyl acetate, washed with water, then brine and dried over Na2SO4. 3-Methoxy-4-chloroaniline was obtained upon concentration and was purified further by column chromatography.

后处理

  1. temperatureAfter cooling to RT
  2. extractionextracted by ethyl acetate
  3. washwashed with water
  4. dry with materialbrine and dried over Na2SO4

来源与证据

ORD记录
ord-e7a1884c2443436e84f576c317dc7d0d
来源数据集
uspto-grants-2008_09
专利号
US07420055B2

关联笔记

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