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Methanol → HCID 54387319, 화합물

HRID 46619
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HRID 46619 반응식
[N+:1]([C:4]1[S:8][C:7]([S:9][C:10]2[CH:15]=[N:14][CH:13]=[CH:12][N+:11]=2[O-:16])=[N:6][CH:5]=1)([O-:3])=[O:2].ClC1C=CC=C(C(OO)=[O:25])C=1.CO>C(Cl)(Cl)Cl>[N+:1]([C:4]1[S:8][C:7]([S:9]([C:10]2[CH:15]=[N:14][CH:13]=[CH:12][N+:11]=2[O-:16])=[O:25])=[N:6][CH:5]=1)([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 70297m-Chloroperbenzoic acidHCID 329658((5-Nitro-2-thiazolyl)thio)pyrazine 1-oxide

생성물 1

HCID 54387319HCID 54387319, 화합물수율 28%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a stirred solution of 1.0 g (0.004 mol) of Compound 2 in 50 ml of chloroform was gradually added 2.0 g (0.010 mol) of 85% m-chloroperbenzoic acid. The reaction mixture was stirred overnight at room temperature and then filtered. The filtrate was washed with water, dilute bicarbonate and brine, and dried over MgSO4. Evaporation of the solvent afforded a yellow oil that solidified on standing. This crude product was recrystallized from CHCl3 /hexane and a second crop of crystals was recrystallized from methanol for a total yield of 0.3 g (28% yield) of yellow crystals, m.p. 139°-141° C.

후처리

  1. filtrationfiltered
  2. washThe filtrate was washed with water, dilute bicarbonate and brine
  3. dry with materialdried over MgSO4
  4. customEvaporation of the solvent
  5. customafforded a yellow oil that solidified
  6. customThis crude product was recrystallized from CHCl3 /hexane

출처 및 근거

ORD 기록
ord-a9f0f356524647c6b03873227f24f8d3
출처 데이터셋
uspto-grants-1979_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04174394

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