HRID1284295

反应详情

EQUATION

反应方程式

HRID 1284295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 9-methylaminoxanthen (5 g.) in dry benzene (10 ml.) was added slowly to a stirred solution of silicon tetraisocyanate (1.16 g.) in benzene (10 ml.). The resulting solution was refluxed for 45 minutes and then evaporated to dryness in vacuo. The residue was refluxed for 30 minutes with 90% isopropanol (20ml.), filtered and the filtrate evaporated to dryness. The residue was washed with cold acetone and recrystallised from ethanol to give N-methyl-N-9-xanthenylurea, m.p. 199°-202°C.

WORKUP

后处理

  1. temperatureThe resulting solution was refluxed for 45 minutes
  2. customevaporated to dryness in vacuo
  3. temperatureThe residue was refluxed for 30 minutes with 90% isopropanol (20ml.)
  4. filtrationfiltered
  5. customthe filtrate evaporated to dryness
  6. washThe residue was washed with cold acetone
  7. customrecrystallised from ethanol