反応 #91172

ord-a280cbbb94b44d6c87a7459224c1758d

反応方程式

O=S(=O)(O)O
Sulfuric acid
CCOC(=O)CC(=O)CCl
ethyl 4-chloroacetoacetate
Oc1ccc(F)c(O)c1F
2,4-difluororesorcinol
O=c1cc(CCl)c2cc(F)c(O)c(F)c2o1
title compound
収率 24.0%
O=c1cc(CCl)c2cc(F)c(O)c(F)c2o1
4-chloromethyl-6,8-difluoro-7-hydroxy-2-chromenone
収率 24.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The precipitate was filtered
  2. 2
    洗浄washed with water
  3. 3
    その他dried by nitrogen gas

実験手順

Sulfuric acid (2 mL) in a flask was cooled to 0° C. After ethyl 4-chloroacetoacetate (0.62 g, 3.8 mmol) was added thereto, 2,4-difluororesorcinol (0.5 g, 3.4 mmol) was added dropwise thereto. The mixture was stirred at room temperature for 2 hours, and the reactant was placed in ice water. The precipitate was filtered, washed with water, and dried by nitrogen gas to obtain the title compound (0.2 g, 24%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09447044B2uspto-grants-2016_09