Guanidine Hydrochloride → Zidovudine guanidine

HRID 273875

反応式

HRID 273875 の反応式
[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]

参加物

5

反応物 3

HCID 5742Guanidine HydrochlorideHCID 14798Sodium HydroxideHCID 35370Zidovudine

生成物 1

HCID 15817654Zidovudine guanidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-376241f84b824599b5aa7c407f3d20bb
出典データセット
uspto-grants-1995_02
特許番号
US05387677

関連ノート

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