2-Isopropylpyridine → 1-Oxo-2-(propan-2-yl)-1lambda~5~-pyridine

HRID 471193

반응식

HRID 471193 반응식
C1C=C(Cl)C=C(C(OO)=[O:9])C=1.[CH:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=1)([CH3:14])[CH3:13]>C(Cl)Cl>[CH:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][N+:16]=1[O-:9])([CH3:14])[CH3:13]

참가 물질

4

반응물 2

HCID 695232-IsopropylpyridineHCID 70297m-Chloroperbenzoic acid

생성물 1

HCID 131720791-Oxo-2-(propan-2-yl)-1lambda~5~-pyridine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

MCPBA (22.0 g) was added to a solution of 2-isopropylpyridine (example 85, step a) (9.1 g) in DCM (250 mL) and the resulting mixture stirred for 3 h. The reaction mixture was washed with saturated sodium bicarbonate solution (4×100 mL) and brine (100 mL), then dried over sodium sulphate, filtered and evaporated. Purification was by silica gel chromatography eluting with ethyl acetate to 10% methanol in ethyl acetate gradient. The fractions containing product were combined and evaporated to give the subtitled compound as a yellow oil. Yield 3.9 g.

후처리

  1. washThe reaction mixture was washed with saturated sodium bicarbonate solution (4×100 mL) and brine (100 mL)
  2. dry with materialdried over sodium sulphate
  3. filtrationfiltered
  4. customevaporated
  5. customPurification
  6. washeluting with ethyl acetate to 10% methanol in ethyl acetate gradient
  7. additionThe fractions containing product
  8. customevaporated

출처 및 근거

ORD 기록
ord-e39c48304864493484370eb858b53aa8
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629271B2

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