反应 #1563928

ord-b3c284283c8b44a29a94ea6296fbbfad

反应方程式

c1ccncc1
Pyridine
CNOC.Cl
N,O-dimethylhydroxylamine hydrochloride
O=C(Cl)CCCCl
Chlorobutyrylchloride
CON(C)C(=O)CCCCl
title compound
收率 93.0%
CON(C)C(=O)CCCCl
4-chloro-N-methoxy-N-methylbutanamide
收率 93.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGwas stirred continuously at 0° C. for 2 h
  2. 2
    洗涤the organic layer was washed with water
  3. 3
    其他The organic layer was separated
  4. 4
    干燥dried over anhydrous sodium sulphate
  5. 5
    浓缩concentrated under reduced pressure

实验过程

Pyridine (101.28 g, 106.6 mL 1281.79 mmol) was added to a solution of N,O-dimethylhydroxylamine hydrochloride (50 g, 512.72 mmol) in DCM (800 mL) at 0° C. and stirring was continued for 15 min. Chlorobutyrylchloride (72.29 g, 512.72 mmol) was then added to this mixture and was stirred continuously at 0° C. for 2 h. The reaction mixture was diluted with DCM and the organic layer was washed with water followed by brine. The organic layer was separated; dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford 79 g of the title compound as a pale brown liquid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09402833B2uspto-grants-2016_08