反应 #1885068

ord-43369921f7354f67af9c5781a203ee67

反应方程式

NC=O
Formamide
COCCOc1cc(N)c(C(=O)OC)cc1OCCOC
compound 21
COCCOc1cc(N)c(C(=O)OC)cc1OCCOC
methyl 2-amino-4,5-bis(2-methoxyethoxy)benzoate
COCCOc1cc2nc[nH]c(=O)c2cc1OCCOC
compound 22
COCCOc1cc2nc[nH]c(=O)c2cc1OCCOC
6,7-bis(2-methoxyethoxy)quinazolin-4(3H)-one

反应条件

温度
167.5°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Reaction
  2. 2
    workup.ADDITIONThe reaction mixture was poured in to ice cold water and solids
  3. 3
    过滤were filtered
  4. 4
    其他The crude product was purified by column chromatography

实验过程

Formamide (130 mL) was added to a solution of compound 21 (13.0 g, 43.43 mmol) in N-methyl-2-pyrrolidone (130 mL) and the reaction mixture was heated to 165-170° C. under N2 for 12 h. Reaction was monitored by TLC. After 8.0 h TLC indicated no starting material. The reaction mixture was poured in to ice cold water and solids were filtered. The crude product was purified by column chromatography to give compound 22 as light yellow solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08343950B2uspto-grants-2013_01