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Sodium Sulfite → HCID 22316883, 화합물

HRID 497291
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HRID 497291 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:12][C:11]([CH3:13])=[N:10][C:9]=2[C:14]2[CH:19]=[CH:18][C:17](SC)=[CH:16][CH:15]=2)=[CH:4][CH:3]=1.[CH:22]1C=C(Cl)C=C(C(OO)=O)C=1.[O-:33][S:34]([O-:36])=O.[Na+].[Na+]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[S:12][C:11]([CH3:13])=[N:10][C:9]=2[C:14]2[CH:15]=[CH:16][C:17]([S:34]([CH3:22])(=[O:36])=[O:33])=[CH:18][CH:19]=2)=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 22316705HCID 22316705, 화합물

생성물 1

HCID 22316883HCID 22316883, 화합물수율 76%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 5-(4-bromophenyl)-2-methyl-4-[4-(methylthio)phenyl]-1,3-thiazole from step 3 (3.8 g, 0.010 mol) in CH2Cl2 (40 mL), m-CPBA (6.2 g, 0.025 mol) was added at 0° C. The mixture was allowed to warm to room temperature and stirred for 12 hours. The mixture was poured into aqueous saturated Na2SO3 (40 mL) and diluted with CH2Cl2 (50 mL). Organic later was separated and washed with aqueous saturated NaHCO3 (50 mL), dried over MgSO4, and concentrated in vacuo. The mixture was purified by flash chromatography eluting with ethyl acetate/hexane (1/1) to give title compound (3.1 g, 76%).

후처리

  1. customOrganic later was separated
  2. washwashed with aqueous saturated NaHCO3 (50 mL)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe mixture was purified by flash chromatography
  6. washeluting with ethyl acetate/hexane (1/1)

출처 및 근거

ORD 기록
ord-53737608f1084cd789531026321768fc
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06949536B2

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