huagongshe.com
HRID53060

反应详情

EQUATION

反应方程式

HRID 53060 的结构方程式

REACTANTS

反应物

2
结构：O=C(O)C(F)(F)F
HCID6422

未命名化合物

结构：CCC(=O)O[C@]1(C(=O)C(O)OC(=O)[C@@H](NC(=O)OC(C)(C)C)C(C)C)CC[C@H]2[C@@H]3C[C@H](C)C4=CC(=O)C=C[C@]4(C)[C@H]3[C@@H](O)C[C@@]21C
HCID86750656

未命名化合物

PRODUCTS

生成物

1
结构：CCC(=O)O[C@]1(C(=O)C(O)OC(=O)[C@@H](N)C(C)C)CC[C@H]2[C@@H]3C[C@H](C)C4=CC(=O)C=C[C@]4(C)[C@H]3[C@@H](O)C[C@@]21C.O=C(O)C(F)(F)F
HCID86750654

未命名化合物

收率 80%

PROCEDURE

实验过程

Under initial cooling, 5 ml of trifluoroacetic acid is poured over 896 mg (1.42 mmol) of N-(1,1-dimethylethoxycarbonyl)valine [11β,21-dihydroxy-3,20-dioxo-6α-methyl-17-propionyloxy-pregna-1,4-dien-21-yl] ester, and it is stirred for 1-2 hours at room temperature. Then, the trifluoroacetic acid is evaporated in a vacuum. The residue is taken up in a little dichloromethane, 5 ml of toluene is added and then evaporated to dryness in a vacuum. The residue is crystallized. 728 mg (80%) of valine [11β,21-dihydroxy-3,20-dioxo-6α-methyl-17-propionyloxy -pregna-1,4-dien-21-yl] ester trifluoroacetate is obtained. Melting point 148° C.

WORKUP

后处理

  1. temperatureUnder initial cooling
  2. customThen, the trifluoroacetic acid is evaporated in a vacuum
  3. additionis added
  4. customevaporated to dryness in a vacuum
  5. customThe residue is crystallized