反应详情

温度

75 °C

A mixture of water (90 mL) and 32% hydrochloric acid (31.4 g) was heated at 75° C. 3'-azido-3'-deoxythymidine-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 3'-azido-3'-deoxythymidine 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 3'-azido-3'-deoxythymidine-guanidine complex suitable for recycling (i.e. acidification).

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