HRID2197395

反应详情

EQUATION

反应方程式

HRID 2197395 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 1000 mL round-bottomed flask was suspended (8S,9S,10R,11S,13S,14S,17R)-11,17-dihydroxy-17-(2-hydroxyacetyl)-10,13-dimethyl-6,7,8,9,10,11,12,13,14,15,16,17-dodecahydro-1H-cyclopenta[a]phenanthren-3(2H)-one (10.4 g, 28.69 mmol) in MeOH (200 mL) and a solution of orthoperiodic acid (9.81 g, 43.04 mmol) in water (200 mL) was added to give a colorless solution. The mixture was stirred for 45 minutes after which an additional 3 g of orthoperiodic acid was added and stirring was continued for another hour. MeOH was removed in vacuo and the residual aqueous mixture was diluted with 200 ml of water. The resulting solid was isolated by filtration and was air-dried on the sinter to yield 8.1 g of the desired compound as a white solid. APCI-MS m/z: 349 [MH+].

WORKUP

后处理

  1. customIn a 1000 mL round-bottomed flask was suspended
  2. customto give a colorless solution
  3. additionwas added
  4. waitwas continued for another hour
  5. customMeOH was removed in vacuo
  6. additionthe residual aqueous mixture was diluted with 200 ml of water
  7. customThe resulting solid was isolated by filtration
  8. customwas air-dried on the sinter