HRID1626652

反应详情

EQUATION

反应方程式

HRID 1626652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of (S)-4-(2-chloro-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-4-yl)-3-methylmorpholine (intermediate 6) as a TFA salt (820 mg, 2.0 mmol) in anhydrous THF (5 ml) was added anhydrous acetone (500 μl) and glacial acetic acid (four drops). The reaction was stirred at RT for 30 minutes after which time sodium triacetoxyborohydride (848 mg, 4.0 mmols) was added. After stirring for a further 30 minutes at RT, the reaction was partitioned between water and DCM. The aqueous phase was extracted into DCM and the organic extracts were combined, dried over magnesium sulphate and concentrated in vacuo to afford the title compound as a brown oil, which was used without further purification.

WORKUP

后处理

  1. additionwas added
  2. customthe reaction was partitioned between water and DCM
  3. extractionThe aqueous phase was extracted into DCM
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated in vacuo