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HRID440428

反应详情

EQUATION

反应方程式

HRID 440428 的结构方程式

REACTANTS

反应物

2
结构：Cl
HCID313

Hydrochloric Acid

ClH

2 次

结构：Cc1cn([C@H]2C[C@H](N=[N+]=[N-])[C@@H](CO)O2)c(=O)[nH]c1=O.N=C(N)N
HCID15817654

未命名化合物

PRODUCTS

生成物

1
结构：Cc1cn([C@H]2C[C@H](N=[N+]=[N-])[C@@H](CO)O2)c(=O)[nH]c1=O
HCID35370

3'-Azido-3'-deoxythymidine

C10H13N5O4

收率 83.6%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

A mixture of water (90 mL) and 32% hydrochloric acid (31.4 g) was heated at 75° C. Zidovudine-guanidine complex (90 g) from Example 1 was added in portions to the aqueous solution and when the addition was completed the pH was 7.56. Thereafter, the pH was adjusted to 1.0 by further addition of 32% hydrochloric acid. The mixture was cooled and crystals formed spontaneously. After several hours the crystals were filtered to yield 61.64 g of crude zidovudine suitable for final purification. 50% caustic (22 g) was added to the mother liquor and a precipitate formed. After 30 minutes the precipitate was filtered to yield 7.99 g zidovudine-guanidine complex suitable for recycling (i.e. acidification).

WORKUP

后处理

  1. additionthe addition
  2. temperatureThe mixture was cooled
  3. customcrystals formed spontaneously
  4. filtrationAfter several hours the crystals were filtered