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HRID918401

反应详情

EQUATION

反应方程式

HRID 918401 的结构方程式

REACTANTS

反应物

4
结构：NC(N)=O
HCID1176

Urea

CH4N2O

结构：CCOCC
HCID3283

Diethyl Ether

C4H10O

结构：C[C@]12C=CC(=O)C=C1CC[C@@H]1[C@@H]2[C@@H](O)C[C@@]2(C)[C@H]1C[C@@H](O)[C@]2(O)C(=O)CO
HCID11047056

16alpha-Hydroxyprednisolone

C21H28O6

结构：[N-]=[N+]=CCOC1CCCCO1
HCID21520879

2-(2-Diazoethoxy)oxane

C7H12N2O2

PRODUCTS

生成物

2
结构：CC(=O)[O-]
HCID175

Acetate

C2H3O2-

结构：C[C@]12C=CC(=O)C=C1CC[C@@H]1[C@@H]2[C@@H](O)C[C@@]2(C)[C@H]1C[C@@H](OCCOC1CCCCO1)[C@]2(O)C(=O)CO
HCID22791775

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

A solution of 2-(tetrahydropyran-2-yloxy)-1-diazoethane (prepared from 69.1 g of N-]2-(tetrahydropyran-2-yloxy)ethyl]urea by the procedure described in (a) - (e) above) in 600 ml of 3:1 ether-pentane is stirred with 200 ml each of ether and methanol at 0°C. Fourteen g of 11β,16α,17,21-tetrahydroxypregna-1,4-diene-3,20-dione, 16,17-cycloborate is added in portions. After nitrogen evolution ceases the solvents are removed in vacuo and the residue is dissolved in chloroform and chromatographed on a 150 g-silica gel column. Elution with chloroform and then 1:1 chloroformethyl acetate gives 4.0 g of TLC pure 16α-[2-(tetrahydropyran-2-yloxy)ethoxy]-11β,17,21-trihydroxypregna-1,4-diene-3,20-dione.

WORKUP

后处理

  1. customare removed in vacuo
  2. dissolutionthe residue is dissolved in chloroform
  3. customchromatographed on a 150 g-silica gel column
  4. washElution with chloroform