m-Chloroperbenzoic acid → HCID 86696139, 화합물

HRID 1426004노트

반응식

HRID 1426004 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[CH:18]=[CH:17][C:16]([C@@H:19]([N:21]2[CH2:26][CH2:25][C:24]([CH2:31][CH:32]3[CH2:34][CH2:33]3)([CH2:27][C:28]([CH3:30])=[CH2:29])[O:23][C:22]2=[O:35])[CH3:20])=[CH:15][CH:14]=1>C(Cl)Cl>[Br:12][C:13]1[CH:18]=[CH:17][C:16]([C@@H:19]([N:21]2[CH2:26][CH2:25][C:24]([CH2:31][CH:32]3[CH2:34][CH2:33]3)([CH2:27][C:28]3([CH3:30])[CH2:29][O:9]3)[O:23][C:22]2=[O:35])[CH3:20])=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 66735700HCID 66735700, 화합물

생성물 1

HCID 86696139HCID 86696139, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

m-Chloroperbenzoic acid (455 mg) was added to a solution of 3-[(S)-1-(4-bromophenyl)-ethyl]-6-(cyclopropylmethyl)-6-(2-methylallyl)-1,3-oxazinan-2-one (516 mg) in CH2Cl2 (15 mL) at 0° C. The mixture was stirred at room temperature overnight. The mixture was then washed with 3% aqueous Na2S2O3 solution and saturated aqueous NaHCO3 solution. The aqueous washing phase was extracted with ethyl acetate (3×30 mL) and the combined organic layer was washed with brine, dried (Na2SO4), and concentrated to afford the crude title compound which was used without further purification. Yield: 490 mg (91% of theory).

후처리

  1. washThe mixture was then washed with 3% aqueous Na2S2O3 solution and saturated aqueous NaHCO3 solution
  2. extractionThe aqueous washing phase was extracted with ethyl acetate (3×30 mL)
  3. washthe combined organic layer was washed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-368f1675a7e1459ab3e5b13c78223d12
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933072B2

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