反応 #4017

ord-7628ca281c8a4d939d7e63b118d19a45

反応方程式

CCOC(CCl)(OCC)OCC
2-chloro-1,1,1-triethoxyethane
Nc1ccccc1S
2-aminothiophenol
ClCc1nc2ccccc2s1
2-chloromethylbenzothiazole
収率 91.3%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄the resulting solution was washed with 3N HCl (10 ml)
  2. 2
    その他The organic portion was evaporated
  3. 3
    その他the residue chromatographed over silica gel

実験手順

A solution of 2-chloro-1,1,1-triethoxyethane (5.9 g) and 2-aminothiophenol (2.5 g) was heated at 80° C. for 15 minutes. After cooling to room temperature, it was dissovled in methylene chloride (30 ml) and the resulting solution was washed with 3N HCl (10 ml) and then with water (20 ml). The organic portion was evaporated and the residue chromatographed over silica gel to obtain 2-chloromethylbenzothiazole (3.35 g; 90% yield), m.p. 34° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04723010uspto-grants-1988_02