Dichloromethane → HCID 68670764, 화합물

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O[CH2:2][C:3]1[CH:4]=[C:5]([C:11](O)([CH3:13])[CH3:12])[C:6]([CH3:10])=[N:7][C:8]=1[CH3:9].C(Cl)[Cl:16]>>[Cl:16][CH2:2][C:3]1[C:8]([CH3:9])=[N:7][C:6]([CH3:10])=[C:5]([C:11]([CH3:13])=[CH2:12])[CH:4]=1

참가 물질

반응물 2

HCID 6344Dichloromethane

HCID 68670777HCID 68670777, 화합물

생성물 1

HCID 68670764HCID 68670764, 화합물

실험 절차

To a stirring solution of 2-(5-(hydroxymethyl)-2,6-dimethylpyridin-3-yl)propan-2-ol in 10 mL of CH2Cl2 was added 1.5 mL of SO2Cl2. After 11 h at r.t., the solution was concentrated and CH2Cl2 and 10 mL of sat. NaHCO3 solution were added, and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated. Purification by flash silica gel chromatography (20% Et2O/hexanes) provided 96.5 mg of the desired 3-(chloromethyl)-2,6-dimethyl-5-(prop-1-en-2-yl)pyridine as a mixture.

후처리

concentrationthe solution was concentrated
additionCH2Cl2 and 10 mL of sat. NaHCO3 solution were added
customthe layers were separated
washThe organic layer was washed with brine
dry with materialdried over Na2SO4
filtrationfiltered
concentrationconcentrated
customPurification by flash silica gel chromatography (20% Et2O/hexanes)

출처 및 근거

ORD 기록: ord-74c2ebecbf054444940569c65eedfc13
출처 데이터셋: uspto-grants-2012_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08299267B2

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