HRID2214757

反应详情

EQUATION

反应方程式

HRID 2214757 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of D2 (1.48 g, 4.9 mmole) in MeOH (50 ml) at room temperature under Ar was treated with aqueous formaldehyde (2.4 ml of 37% w/v, 29 mmole), followed by portionwise addition of NaBH3CN (920 mg, 15 mmole). The mixture was stirred at room temperature for 3 h, then concentrated under vacuum and the residue treated with 10% Na2CO3 solution and extracted with DCM. The extract was dried (Na2SO4) and concentrated under vacuum to afford the title compound as a yellow solid (1.4 g, 90%). MH+ 318.

WORKUP

后处理

  1. concentrationconcentrated under vacuum
  2. additionthe residue treated with 10% Na2CO3 solution
  3. extractionextracted with DCM
  4. dry with materialThe extract was dried (Na2SO4)
  5. concentrationconcentrated under vacuum