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1-Chloroethyl chloroformate → 5-(2-Chlorophenyl)-1,2,3,6-tetrahydropyridine hydrochloride

HRID 2245258
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HRID 2245258 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH2:13][N:12](C)[CH2:11][CH2:10][CH:9]=1.ClC(OC(Cl)C)=O>ClCCl.CO>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH2:13][NH:12][CH2:11][CH2:10][CH:9]=1
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참가 물질

5

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 684186035-(2-Chlorophenyl)-1,2,3,6-tetrahydro-1-methylpyridine

생성물 1

HCID 684184535-(2-Chlorophenyl)-1,2,3,6-tetrahydropyridine hydrochloride수율 73.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To a solution of the 5-(2-chlorophenyl)-1,2,3,6-tetrahydro-1-methylpyridine (5.9 g) in dichloromethane (60 ml) was added 1-chloroethyl chloroformate (5.1 ml) and the mixture was stirred for 2.5 h. The mixture was washed with water and then with a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give brown oil. A solution of the obtained oil in methanol was refluxed for 2 h. The solvent was evaporated under reduced pressure and the obtained residue was crystallized from ethyl acetate to give 5-(2-chlorophenyl)-1,2,3,6-tetrahydropyridine hydrochloride (2.4 g). A solution of 5-(2-chlorophenyl)-1,2,3,6-tetrahydropyridine hydrochloride (156 mg), 2-chloro-1,6-dihydro-1-methyl-6-oxo-4-(pyridin-4-yl)pyrimidine (150 mg) and triethylamine (236 μl) in dimethylformamide (3 ml) was stirred at room temperature for 6 h. To the reaction mixture was added water (3 ml), and the precipitated crystals were collected by filtration to give the title compound (240 mg) as white crystals.

후처리

  1. washThe mixture was washed with water
  2. dry with materialwith a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customto give brown oil
  5. customThe solvent was evaporated under reduced pressure
  6. customthe obtained residue was crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-9e76839650c443358848b27bac5f2d6b
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07683069B2

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