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HRID743496

反应详情

EQUATION

反应方程式

HRID 743496 的结构方程式

REACTANTS

反应物

3
结构：CCCC=O
HCID261

Butanal

C4H8O

结构：Cc1ccc(S(=O)(=O)O)cc1
HCID6101

4-Methylbenzenesulfonic acid

C7H8O3S

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

PRODUCTS

生成物

1
结构：CCCC1O[C@@H]2C[C@H]3[C@@H]4CCC5=CC(=O)C=C[C@]5(C)[C@H]4[C@@H](O)C[C@]3(C)[C@]2(C(=O)CO)O1
HCID5281004

Budesonide

C25H34O6

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC#N
溶剂HCID6342

Acetonitrile

C2H3N

PROCEDURE

实验过程

The reaction is carried out in a nitrogen atmosphere. 15,4 g p-toluenesulphonic acid is dissolved into 200 ml acetonitrile. To the solution 50,0 g 16α-hydroxyprednisolone and 17.6 ml butanal are added. The temperature rises to 25° C. After 30 min most of the material is dissolved. Shortly thereafter the product starts to crystallize. After 3 hours the reaction is stopped by the addition of 75 ml aqueous saturated sodium hydrogen carbonate solution, whereupon the product crystallizes. The dried product is dissolved in methylene chloride and methanol and is crystallized by the addition of ligroine (b.p. 40-65) giving crude budesonide.

WORKUP

后处理

  1. customrises to 25° C
  2. dissolutionAfter 30 min most of the material is dissolved
  3. customto crystallize
  4. additionAfter 3 hours the reaction is stopped by the addition of 75 ml aqueous saturated sodium hydrogen carbonate solution, whereupon the product
  5. customcrystallizes
  6. dissolutionThe dried product is dissolved in methylene chloride
  7. custommethanol and is crystallized by the addition of ligroine (b.p. 40-65)