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m-Chloroperbenzoic acid → HCID 59743399, 화합물

HRID 1946995
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HRID 1946995 반응식
ClC1C=C(C=CC=1)C(OO)=[O:6].[CH3:12][S:13][C:14]1[N:19]=[C:18]([N:20]2[C:28]3[C:23](=[C:24]([N+:29]([O-:31])=[O:30])[CH:25]=[CH:26][CH:27]=3)[CH:22]=[CH:21]2)[CH:17]=[CH:16][N:15]=1>C(Cl)(Cl)Cl.C(Cl)Cl>[CH3:12][S:13]([C:14]1[N:19]=[C:18]([N:20]2[C:28]3[C:23](=[C:24]([N+:29]([O-:31])=[O:30])[CH:25]=[CH:26][CH:27]=3)[CH:22]=[CH:21]2)[CH:17]=[CH:16][N:15]=1)=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 59743448HCID 59743448, 화합물

생성물 1

HCID 59743399HCID 59743399, 화합물수율 55.8%

시약·촉매·용매 2

HCID 6212Chloroform용매2회HCID 6344Dichloromethane용매

실험 절차

A suspension of 3-chloroperoxybenzoic acid (77%, 3.11 g) in CHCl3 (40 mL) was slowly added at 0° C. under N2 to a mixture of 1-(2-methylsulfanylpyrimidin-4-yl)-4-nitro-1H-indole (3.93 g, 14.0 mmol) in CHCl3 (50 mL). The resulting mixture was allowed to warm up to RT, and stirred overnight. The reaction mixture was then diluted with DCM (200 mL) and washed with aqueous NaHCO3 (saturated). The resulting yellow precipitate was collected by filtration and dried under reduced pressure to give 1-(2-methanesulfinyl-pyrimidin-4-yl)-4-nitro-1H-indole (2.36 g). The mother liquors were dried over Na2SO4, filtered and evaporated under reduced pressure to give a second aliquot (690 mg).

후처리

  1. washwashed with aqueous NaHCO3 (saturated)
  2. filtrationThe resulting yellow precipitate was collected by filtration
  3. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-10c1f5864a414572a02ec046da1dfa0e
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399462B2

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