Peracetic Acid → Sufotidine

HRID 652099ノート

反応式

HRID 652099 の反応式
[C:1](OO)(=O)C.[CH3:6][N:7]1[C:11]([NH:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][N:24]3[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]3)[CH:18]=2)=[N:10][C:9]([CH2:30]SC)=[N:8]1.C([O-])(=O)C.[Na+].[S:38]([O-:41])([O-])=[O:39].[Na+].[Na+]>C(O)(=O)C>[CH3:6][N:7]1[C:11]([NH:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][N:24]3[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]3)[CH:18]=2)=[N:10][C:9]([CH2:30][S:38]([CH3:1])(=[O:41])=[O:39])=[N:8]1

参加物

6

反応物 4

HCID 6585Peracetic AcidHCID 24437Sodium SulfiteHCID 517045Sodium AcetateHCID 12774362HCID 12774362、化合物

生成物 1

HCID 71763Sufotidine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

Peracetic acid (1.05 ml of a 6.1M solution) in acetic acid (7 ml) was added to an ice-cooled solution of 1-methyl-3-methylthiomethyl-N-[3-[3-(1-piperidinylmethyl)phenoxy]propyl]-1H-1,2,4-triazole-5-amine (0.82 g) in acetic acid (10 ml) with sodium acetate (0.52 g). The mixture was stirred at room temperature for 18 h, sodium sulphite (1.25 g) added and the mixture evaporated to dryness. The residue was basified to pH 8 with sodium bicarbonate solution, washed with ethyl acetate, basified to pH 10 with sodium carbonate and extracted with ethyl acetate to give a foam (0.46 g). This was crystallised from methyl acetate-petroleum ether (b.p. 60°-80°) to give the title compound as a white solid (0.22 g), m.p. 121°-122°.

後処理

  1. customthe mixture evaporated to dryness
  2. washwashed with ethyl acetate
  3. extractionextracted with ethyl acetate

出典と根拠

ORDレコード
ord-57631e0af2e6456ca896df9b00a129e3
出典データセット
uspto-grants-1987_06
特許番号
US04670448

反応ノート

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