반응 #5883

ord-6cc07c4d63d84829877b5eb5f5957d9d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도maintaining the temperature at 0°-2°
  2. 2
    여과The solid is filtered
  3. 3
    기타the filtrate is evaporated
  4. 4
    기타The solid thus obtained
  5. 5
    여과filtered through a silica gel column
  6. 6
    기타The filtrate is evaporated

실험 절차

To a cooled mixture of 2.1 g of 6-amino-2-tert-butyl-5-(4-methylpiperidin-1-yl)benzothiazole and 2.8 g of potassium bicarbonate in 20 ml of chloroform is added dropwise 1.6 g of thiophosgene in 5 ml of chloroform under stirring. The stirring is continued for 2 hours maintaining the temperature at 0°-2° . The solid is filtered and the filtrate is evaporated. The solid thus obtained is dissolved in chloroform and filtered through a silica gel column. The filtrate is evaporated to give 2-tert-butyl-6-isothiocyanato-5-(4-methylpiperidin-1-yl)benzothiazole, melting at 54°-58°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246927uspto-grants-1993_09