苯甲酰氯 → Methyl-2-methoxy-5-benzamidobenzoate

HRID 840604笔记

反应方程式

HRID 840604 反应方程式
[CH3:1][O:2][C:3](=[O:13])[C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[CH:6][C:5]=1[O:11][CH3:12].C(N(CC)CC)C.[C:21](Cl)(=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:13])[C:4]1[CH:9]=[C:8]([NH:10][C:21](=[O:28])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:7]=[CH:6][C:5]=1[O:11][CH3:12]

参与物

5

反应物 3

HCID 7412苯甲酰氯HCID 8471三乙胺HCID 898435-氨基-2-甲氧基苯甲酸甲酯

产物 1

HCID 22620052Methyl-2-methoxy-5-benzamidobenzoate

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

反应条件

温度
0 °C

实验过程

A solution of 9.92 grams (55 mmol) of methyl-2-methoxy-5-aminobenzoate was taken up in 250 ml methylene chloride, treated with 8.4 mL (61 mmol) triethylamine and cooled to 0° C. The reaction mixture was then treated with 8.1 grams (57 mmol) benzoyl chloride in a dropwise fashion. The reaction mixture was stirred for 30 minutes while warming to room temperature. The reaction mixture was diluted with 500 mL of methylene chloride, washed with 200 mL saturated bicarbonate solution and then rewashed with water and brine. The organic phase was dried and evaporated to a flaky white solid (15.7 grams). This material was used without further purification.

后处理

  1. temperaturewhile warming to room temperature
  2. washwashed with 200 mL saturated bicarbonate solution
  3. customThe organic phase was dried
  4. customevaporated to a flaky white solid (15.7 grams)
  5. customThis material was used without further purification

来源与证据

ORD记录
ord-ac97a016dea644448e4169f99f7faaeb
来源数据集
uspto-grants-2002_04
专利号
US06369074B1

反应笔记

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