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m-Chloroperbenzoic acid → HCID 54523856, 화합물

HRID 892533
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HRID 892533 반응식
[C:1]([C:9]1[CH:10]=[CH:11][C:12]2[O:17][C:16]([CH3:19])([CH3:18])[CH2:15][CH:14]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[C:13]=2[CH:26]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC1C=CC=C(C(OO)=[O:35])C=1>ClCCl>[C:1]([C:9]1[CH:10]=[CH:11][C:12]2[O:17][C:16]([CH3:19])([CH3:18])[CH2:15][CH:14]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N+:21]=3[O-:35])[C:13]=2[CH:26]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 19895648HCID 19895648, 화합물

생성물 1

HCID 54523856HCID 54523856, 화합물수율 20.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

94 mg of 6-benzoyl-3,4-dihydro-2,2-dimethyl-4-(2-pyridyl)-2H-1-benzopyran and 52 mg of m-chloroperbenzoic acid were stirred in 15 ml of dichloromethane at room temperature until thin-layer chromatography indicated that the reaction was complete. The mixture was washed in succession with sodium bisulphite solution and sodium bicarbonate solution, then dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using 10% (v/v) methanol/ethyl acetate for the elution. After trituration with diethyl ether there were obtained 20 mg of 2-(6-benzoyl-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-4-yl)pyridine N-oxide of melting point 134°-136° C.

후처리

  1. washThe mixture was washed in succession with sodium bisulphite solution and sodium bicarbonate solution
  2. dry with materialdried over sodium sulphate
  3. customevaporated
  4. customThe residue was chromatographed on silica gel using 10% (v/v) methanol/ethyl acetate for the elution

출처 및 근거

ORD 기록
ord-0fd587b5eb74471ab290b5d100ca68b2
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05118694

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