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HRID127168

反应详情

EQUATION

反应方程式

HRID 127168 的结构方程式

REACTANTS

反应物

3
结构：c1ccccc1
HCID241

Benzene

C6H6

结构：CC(=O)OCC(=O)[C@@]1(O)CC[C@H]2[C@@H]3CCC4=CC(=O)C=C[C@]4(C)[C@@]34O[C@H]4C[C@@]21C
HCID11876290

9beta,11beta-Epoxy-17,21-dihydroxypregna-1,4-diene-3,20-dione 21-acetate

C23H28O6

结构：C=C(C)CC(=O)[O-]
HCID18355900

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)OCC(=O)[C@@]1(O)CC[C@H]2[C@@H]3CC=C4C=C(OC(C)=O)C=C[C@]4(C)[C@@]34O[C@H]4C[C@@]21C
HCID86737547

未命名化合物

PROCEDURE

实验过程

10 g of sulfonic acid resin (Amberlite I R120, marketed by Rohm and Haas Co.) was dehydrated by azeotropic destillation with benzene. The dry resin was suspended in 50 ml isopropenylacetate and 10 g 9β,11β-epoxy-21-acetoxy-17-hydroxy-pregna-1,4-diene-3,20-dione were added. The mixture was heated under reflux for 5 hours, cooled and filtered an the filtrate was evaporated to dryness. The residue which crystallized from methanol (0,5% pyridine) gave in high yield (9,5 grams) 3,21-diacetoxy-17-hydroxy-9β,11β-epoxy-pregna-1,3,5-triene-20-one. Melting point: 194° C., λmax 310 nm (ε5500)⟦alpha⟧sub.D in chloroform -199° C. (c=1% chloroform), νmax (cm-1) (K Br) 3450; 1765; 1740; 1725; 1655; 1625; 1590.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. temperaturecooled
  4. filtrationfiltered an the filtrate
  5. customwas evaporated to dryness
  6. customThe residue which crystallized from methanol (0,5% pyridine)
  7. customgave