HRID562705

反应详情

EQUATION

反应方程式

HRID 562705 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-(butyloxy)-8-(methyloxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (7.34 g) in methanol (100 ml) was added trifluoroacetic acid (10 ml). The mixture was stirred at ambient temperature over the weekend to give a suspension. The reaction mixture was concentrated to a small volume (thick slurry) before being diluted with ethyl acetate (50 ml). The resultant slurry was filtered and washed with a small volume of ethyl acetate until the filtrate was colourless. The solid remaining was dried by air and then in vacuo to give the title compound as a white solid (6.20 g). The filtrate obtained previously was concentrated to give a slurry which was diluted with a small volume of ethyl acetate (10 ml) and then filtered and dried as above. This second crop was isolated as a white solid (0.276 g). Both crops were identical by NMR.

WORKUP

后处理

  1. customto give a suspension
  2. concentrationThe reaction mixture was concentrated to a small volume (thick slurry)
  3. additionbefore being diluted with ethyl acetate (50 ml)
  4. filtrationThe resultant slurry was filtered
  5. washwashed with a small volume of ethyl acetate until the filtrate
  6. customThe solid remaining was dried by air