反応 #1552087

ord-39636d1a06cd44efa85961acb947f4ec

反応方程式

Cn1nc(C(F)F)c(C(=O)O)c1Cl
5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid
O=S(Cl)Cl
thionyl chloride
Cn1nc(C(F)F)c(C(=O)Cl)c1Cl
5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling down
  2. 2
    その他the reaction mixture is evaporated under vacuum

実験手順

3.2 g of 5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid and 44.3 ml of thionyl chloride are refluxed for 5 hours. After cooling down, the reaction mixture is evaporated under vacuum to yield 3.5 g of 5-chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride as a yellow oil. 1H NMR (400 MHz, CHCl3-d6) δ ppm: 3.97 (s, 3H); 7.00 (t, J=52.01 Hz, 1H); IR (TQ): 1759 and 1725 cm−1 (C═O).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08999956B2uspto-grants-2015_04