Sodium Dithionite → 4,5-Diamino-2-benzylpyrimid-6-one

HRID 1288278ノート

反応式

HRID 1288278 の反応式
S(S([O-])=O)([O-])=O.[Na+].[Na+].[NH2:9][C:10]1[N:11]=[C:12]([CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[NH:13][C:14](=[O:24])[C:15]=1[N:16]=NC1C=CC=CC=1>O.CN(C)C=O>[NH2:9][C:10]1[N:11]=[C:12]([CH2:25][C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[NH:13][C:14](=[O:24])[C:15]=1[NH2:16]

参加物

5

反応物 2

HCID 24489Sodium DithioniteHCID 1363546174-Amino-2-benzyl-5-phenylazopyrimid-6-one

生成物 1

HCID 1363546164,5-Diamino-2-benzylpyrimid-6-one収率 64.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of sodium dithionite (62 g.) in water (300 ml.) was added dropwise during 30 minutes to a solution of 4-amino-2-benzyl-5-phenylazopyrimid-6-one (27 g.) in dimethylformamide (1000 ml.) at 75° C. The mixture was cooled, and the insoluble solid was filtered off. The filtrate was evaporated in vacuo, the residue was stirred with water, and the solid filtered off. This solid was extracted with boiling water (250 ml.), the extract was filtered hot and then cooled. The solid which separated was recrystallised from water to give 4,5-diamino-2-benzylpyrimid-6-one (12.4 g.) in the form of off-white needles, m.p. 243° C. (with decomposition).

後処理

  1. temperatureThe mixture was cooled
  2. filtrationthe insoluble solid was filtered off
  3. customThe filtrate was evaporated in vacuo
  4. filtrationthe solid filtered off
  5. extractionThis solid was extracted with boiling water (250 ml.)
  6. filtrationthe extract was filtered hot
  7. temperaturecooled
  8. customThe solid which separated
  9. customwas recrystallised from water

出典と根拠

ORDレコード
ord-bdddfab5641e4bbdb20a91ddc14c714f
出典データセット
uspto-grants-1976_10
特許番号
US03987160

反応ノート

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