HRID461803

反应详情

EQUATION

反应方程式

HRID 461803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3-Isothiocyanatopyridine (6.8 g.) is added to a solution of (S)-3-hydroxymethyl-1,2,3,4-tetrahydroisoquinoline (8.15 g.) in ethanol (150 cc.). After 3 hours at a temperature of about 20° C., the solution is cooled to 0° C. The white crystals which have appeared are filtered off and are then recrystallised from propanol (200 cc.). After filtration, the crystals are washed with propanol (2 × 10 cc.) and then dried at 60° C. under reduced pressure (1 mm. Hg). (S)-3-Hydroxymethyl-N-(pyrid-3-yl)-1,2,3,4-tetrahydroisoquinoline-2-carbothioamide (12.1 g.) melting at 192° C is thus obtained.

WORKUP

后处理

  1. filtrationThe white crystals which have appeared are filtered off
  2. customare then recrystallised from propanol (200 cc.)
  3. filtrationAfter filtration
  4. washthe crystals are washed with propanol (2 × 10 cc.)
  5. customdried at 60° C. under reduced pressure (1 mm. Hg)