反応 #685701

ord-8b9c6fe51079404f9f89c6c44a44a38b

反応方程式

Nc1cc(F)c(F)cc1F
2,4,5-trifluoroaniline
CCOC(=S)[S-].[K+]
potassium ethylxanthogenate
Cl
HCl
Fc1cc2nc(S)sc2cc1F
titled compound
収率 40.0%
Fc1cc2nc(S)sc2cc1F
5,6-Difluoro-benzothiazole-2-thiol
収率 40.0%

反応条件

温度
95°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was cooled to room temperature
  2. 2
    ろ過The precipitate was collected by filtration
  3. 3
    洗浄washed with water
  4. 4
    その他dried

実験手順

A mixture of 1 g (6.80 mmol) 2,4,5-trifluoroaniline and 1.33 g (8.16 mmol) potassium ethylxanthogenate in 5 mL dry N,N-dimethylformamide was heated in a 95° C. oil bath for 7 h. The reaction mixture was cooled to room temperature and diluted with water (15 mL). The mixture was acidified with aqueous HCl 2N. The precipitate was collected by filtration, washed with water and dried to provide 0.55 g (40%) of the titled compound as a light yellow solid. MS(m/e): 201.9 (M−H+).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07897627B2uspto-grants-2011_03