Potassium Carbonate → 5-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-methyl-pyrimidin-4-ylamine

HRID 2294004

반응식

HRID 2294004 반응식
Cl.Cl[CH2:3][C:4]1[C:5]([NH2:11])=[N:6][C:7]([CH3:10])=[N:8][CH:9]=1.Cl.[F:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH2:21][CH2:22][NH:23][CH2:24][CH:25]=2)=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH2:25][CH2:24][N:23]([CH2:3][C:4]3[C:5]([NH2:11])=[N:6][C:7]([CH3:10])=[N:8][CH:9]=3)[CH2:22][CH:21]=2)=[CH:16][CH:15]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1977474-(4-Fluorophenyl)-1,2,3,6-tetrahydropyridine hydrochlorideHCID 214736115-(Chloromethyl)-2-methylpyrimidin-4-amine--hydrogen chloride (1/1)

생성물 1

HCID 214736285-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-methyl-pyrimidin-4-ylamine수율 28%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 27.2 g (0.14 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride, 29.8 g (0.14 mol) of 4-(4-fluoro-phenyl)-1,2,3,6-tetrahydropyridine hydrochloride and 42 g (0.30 mol) of dry potassium carbonate in 200 ml of dimethyl-formamide was stirred at room temperature for 18 hours. The mixture was suction filtered, the filter cake was washed with dichloromethane, the filtrate was completely freed from the solvents and the residue was crystallized twice from ethyl acetate/cyclohexane. 11.6 g (28%) of 5-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-methyl-pyrimidin-4-ylamine were obtained as yellowish crystals; m.p. 176°-178°.

후처리

  1. filtrationfiltered
  2. washthe filter cake was washed with dichloromethane
  3. customthe residue was crystallized twice from ethyl acetate/cyclohexane

출처 및 근거

ORD 기록
ord-a6b760196417413bb732954c365e53c3
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05688798

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