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Sodium Sulfite → HCID 22316883, 화합물

HRID 2086735
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HRID 2086735 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 temperrature 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 concentarted 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. temperatureto warm to room temperrature
  2. customOrganic later was separated
  3. washwashed with aqueous saturated NaHCO3 (50 mL)
  4. dry with materialdried over MgSO4
  5. customThe mixture was purified by flash chromatography
  6. washeluting with ethyl acetate/hexane (1/1)

출처 및 근거

ORD 기록
ord-94b40eda78034ec1b761829dfba6bf39
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06727238B2

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