Реакция #5883

ord-6cc07c4d63d84829877b5eb5f5957d9d

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураmaintaining the temperature at 0°-2°
  2. 2
    ФильтрацияThe solid is filtered
  3. 3
    Другоеthe filtrate is evaporated
  4. 4
    ДругоеThe solid thus obtained
  5. 5
    Фильтрацияfiltered through a silica gel column
  6. 6
    ДругоеThe filtrate is evaporated

Методика

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°.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05246927uspto-grants-1993_09