反应 #1583826

ord-d2c6227684bf4edea1dc63c49057823b

反应方程式

COC(=O)NCc1cc(C(=O)C=CN(C)C)ccc1Cl
methyl N-[[2-chloro-5-[3-(dimethylamino)-1-oxo-2-propen-1-yl]phenyl]methyl]carbamate
COC(=O)NCc1cc(C(=O)C=CN(C)C)ccc1Cl
product
COC(=O)NCc1cc(C(=O)C=CN(C)C)ccc1Cl
methyl N-[[2-chloro-5-[3-(dimethylamino)-1-oxo-2-propen-1-yl]phenyl]methyl]carbamate
NN.O
hydrazine hydrate
COC(=O)NCc1cc(-c2cc[nH]n2)ccc1Cl
title compound
COC(=O)NCc1cc(-c2cc[nH]n2)ccc1Cl
methyl N-[[2-chloro-5-(1H-pyrazol-3-yl)phenyl]methyl]carbamate

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The reaction mixture was filtered
  2. 2
    其他the solid collected
  3. 3
    其他was dried under reduced pressure

实验过程

To a solution of methyl N-[[2-chloro-5-[3-(dimethylamino)-1-oxo-2-propen-1-yl]phenyl]methyl]carbamate (i.e. the product of Step A) (4.14 g, 13.9 mmol) in methanol (80 mL) was added hydrazine hydrate (0.771 g, 15.4 mmol). The reaction mixture was stirred at room temperature for 2 days. The reaction mixture was filtered and the solid collected was dried under reduced pressure to provide the title compound, a compound of the present invention, as a solid (3.26 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09198433B2uspto-grants-2015_12