Peracetic Acid → Sufotidine

HRID 652099노트

반응식

HRID 652099 반응식
[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

참가 물질

6

반응물 4

HCID 6585Peracetic AcidHCID 24437Sodium SulfiteHCID 517045Sodium AcetateHCID 12774362HCID 12774362, 화합물

생성물 1

HCID 71763Sufotidine

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록
ord-57631e0af2e6456ca896df9b00a129e3
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04670448

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