Guanidine Hydrochloride → Zidovudine guanidine

HRID 273875

반응식

HRID 273875 반응식
[N:1]([C@@H:4]1[C@@H:8]([CH2:9][OH:10])[O:7][C@@H:6]([N:11]2[CH:19]=[C:17]([CH3:18])[C:15](=[O:16])[NH:14][C:12]2=[O:13])[CH2:5]1)=[N+:2]=[N-:3].[OH-].[Na+].Cl.[NH2:23][C:24]([NH2:26])=[NH:25]>O>[NH2:25][C:24]([NH2:26])=[NH:23].[N:1]([C@@H:4]1[C@@H:8]([CH2:9][OH:10])[O:7][C@@H:6]([N:11]2[CH:19]=[C:17]([CH3:18])[C:15](=[O:16])[NH:14][C:12]2=[O:13])[CH2:5]1)=[N+:2]=[N-:3]

참가 물질

5

반응물 3

HCID 5742Guanidine HydrochlorideHCID 14798Sodium HydroxideHCID 35370Zidovudine

생성물 1

HCID 15817654Zidovudine guanidine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

An analytical grade sample of the 3'-azido-3'-deoxythymidine guanidine salt was prepared by suspending pharmaceutical grade 3'-azido-3'-deoxythymidine (53.4 g) in water (250 mL) and adding 50% sodium hydroxide (17.6 g) to provide a mixture having a pH of 13.0. The mixture was then heated to 70° C. Thereafter, guanidine hydrochloride (23 g) was added as a solid and the mixture was heated to 97° C. to dissolve the emerging precipitate. The mixture was then set aside to cool and crystallize, and it was stirred for 16 hours. Thereafter, the crystals were filtered and washed with water and ethanol to yield 58.76 (90%) of white crystals. The crystals had a melting point of 210.9°-212° C.

후처리

  1. customto provide a mixture
  2. temperaturethe mixture was heated to 97° C.
  3. dissolutionto dissolve the emerging precipitate
  4. temperatureto cool
  5. customcrystallize
  6. filtrationThereafter, the crystals were filtered
  7. washwashed with water and ethanol

출처 및 근거

ORD 기록
ord-376241f84b824599b5aa7c407f3d20bb
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387677

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