反应 #1885071

ord-82eac5a66cfe4c2ab0baa0d0f5b854bc

反应方程式

ClCCl
Dichloromethane
O=C(O)CCCn1c(=O)[nH]c2ccccc21
4-(2-oxo-2,3-dihydrobenzimidazol-1-yl)butyric acid
O=C(Cl)C(=O)Cl
oxalyl chloride
O=C(CCCn1c(=O)[nH]c2ccccc21)OCl
chloro 2,3-dihydro-2-oxo-1H-benzimidazol-1-butanoate

反应条件

温度
10°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGThe resulting mixture was then stirred at 15-20° C. for an additional 1-3 hours

实验过程

Dichloromethane (3772 L) and then 4-(2-oxo-2,3-dihydrobenzimidazol-1-yl)butyric acid (525 kg; 2.4 kmol) were charged to a stirred-tank reactor, followed by N,N-dimethylformamide (21 L). The resulting mixture was cooled to 10° C. Afterward, oxalyl chloride (326.8 kg)) was dosed at 10-15° C. over 2-3 hours while stirring. The resulting mixture was then stirred at 15-20° C. for an additional 1-3 hours. All the above steps were conducted under a N2 atmosphere. Conversion was checked by in-process control (“IPC”).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08343956B2uspto-grants-2013_01