醋酸 → 6-(4-苄基氨基-3-硝基苯基)-5-甲基-2,3,4,5-四氢哒嗪-3-酮

HRID 930552笔记

反应方程式

HRID 930552 反应方程式
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=O)[CH:16]([CH3:21])[CH2:17][C:18](O)=[O:19])=[CH:11][C:10]=1[N+:23]([O-:25])=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:27][NH2:28].C(O)(=O)C>C(O)C>[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]([CH3:21])[CH2:17][C:18](=[O:19])[NH:27][N:28]=2)=[CH:11][C:10]=1[N+:23]([O-:25])=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参与物

5

反应物 3

HCID 176醋酸2 次HCID 24654水合肼2 次HCID 674500244-[4-(Benzylamino)-3-nitrophenyl]-3-methyl-4-oxobutanoic acid

产物 1

HCID 117246806-(4-苄基氨基-3-硝基苯基)-5-甲基-2,3,4,5-四氢哒嗪-3-酮

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

反应条件

温度
100 °C

实验过程

4-(4-Benzylamino-3-nitro-phenyl)-3-methyl-4-oxo-butyric acid E-4.1″ (939 mg; 2.74 mmol) is placed in 7 ml ethanol and treated with hydrazine hydrate (0.16 ml; 3.29 mmol) and acetic acid (78.58 μl; 1.37 mmol). The reaction mixture is heated up to 100° C. for 2 hours. Another portion of hydrazine hydrate (0.08 ml; 1.65 mmol) and 40 μl acetic acid are added and stirred for 2 hours at 100° C. After letting the reaction cooling to RT, the product precipitates. It is filtered off and washed with methanol and dried under reduced pressure.

后处理

  1. temperaturecooling to RT
  2. customthe product precipitates
  3. filtrationIt is filtered off
  4. washwashed with methanol
  5. customdried under reduced pressure

来源与证据

ORD记录
ord-43f285e70cfa4190b1449e64e1717aab
来源数据集
uspto-grants-2016_03
专利号
US09296748B2

反应笔记

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