HRID2395097

反应详情

EQUATION

反应方程式

HRID 2395097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.9 g (5.29 mmol) of benzyl 5-[(1-tert-butoxyformamido)methyl]-3,6-dimethoxy-9,9-dimethylxanthene-4-acetate were taken up in a mixture of 10 ml of trifluoroacetic acid and 5 ml of water at 0°. After half an hour the solvents were removed, whereupon the residue was treated with 20 ml of ether. The resulting solid was filtered off, washed with ether and dried over magnesium sulphate, whereby 2.25 g of benzyl 5-aminomethyl-3,6-dimethoxy-9,9-dimethylxanthene-4-acetate trifluoroacetate were obtained as a colourless powder of m.p. 169.5°-171°; IR 1716, 1662, 1631, 1604, 1538, 1494 cm-1.

WORKUP

后处理

  1. customAfter half an hour the solvents were removed, whereupon the residue
  2. additionwas treated with 20 ml of ether
  3. filtrationThe resulting solid was filtered off
  4. washwashed with ether
  5. dry with materialdried over magnesium sulphate