HRID2197393

反应详情

EQUATION

反应方程式

HRID 2197393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 250 mL round-bottomed flask was suspended (6S,8S,9S,10R,11S,13S,14S,17R)-11,17-dihydroxy-17-(2-hydroxyacetyl)-6,10,13-trimethyl-6,7,8,9,10,11,12,13,14,15,16,17-dodecahydro-3H-cyclopenta[a]phenanthren-3-one (6α-Methylprednisolon, 4.3 g, 11.48 mmol) in EtOAc (80 mL) and the reaction mixture was diluted with ethanol (20.0 mL). Tris(triphenylphosphine)rhodium(I)chloride (Wilkinson's catalyst, 1 g, 1.08 mmol) was added together with a magnetic stirrer bar and the flask was vigorously stirred in a hydrogen atmosphere (1 atm) at room temperature for 1 week. The reaction mixture was filtered through a glass filter funnel and the filtrate was concentrated in vacuo to yield 4.07 g of the desired compound as a light brown solid which was used in the next step without any further purification. APCI-MS m/z: 377 [MH+].

WORKUP

后处理

  1. customIn a 250 mL round-bottomed flask was suspended
  2. filtrationThe reaction mixture was filtered through a glass
  3. filtrationfilter funnel
  4. concentrationthe filtrate was concentrated in vacuo