Hydrochloric Acid → Zidovudine

HRID 440428

반응식

HRID 440428 반응식
Cl.[CH3:2][C:3]1[C:9](=[O:10])[NH:8][C:6](=[O:7])[N:5]([C@@H:11]2[O:15][C@H:14]([CH2:16][OH:17])[C@@H:13]([N:18]=[N+:19]=[N-:20])[CH2:12]2)[CH:4]=1.NC(N)=N>O>[CH3:2][C:3]1[C:9](=[O:10])[NH:8][C:6](=[O:7])[N:5]([C@@H:11]2[O:15][C@H:14]([CH2:16][OH:17])[C@@H:13]([N:18]=[N+:19]=[N-:20])[CH2:12]2)[CH:4]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric Acid2회HCID 15817654Zidovudine guanidine

생성물 1

HCID 35370Zidovudine수율 83.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
75 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-002c043efee7446bbd90f4ece77e4284
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05519129

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