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Potassium Carbonate → HCID 21473645, 화합물

HRID 2294031
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HRID 2294031 반응식
Br.Br.Br[CH2:4][C:5]1[C:6]([NH2:14])=[N:7][C:8]([CH2:11][CH2:12][CH3:13])=[N:9][CH:10]=1.Cl.[F:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH2:24][CH2:25][NH:26][CH2:27][CH:28]=2)=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH2:28][CH2:27][N:26]([CH2:4][C:5]3[C:6]([NH2:14])=[N:7][C:8]([CH2:11][CH2:12][CH3:13])=[N:9][CH:10]=3)[CH2:25][CH:24]=2)=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1977474-(4-Fluorophenyl)-1,2,3,6-tetrahydropyridine hydrochlorideHCID 21473668HCID 21473668, 화합물

생성물 1

HCID 21473645HCID 21473645, 화합물수율 21.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 7.0 g (0.020 mol) of 5-bromomethyl-2-propyl-pyrimidin-4-ylamine dihydrobromide, 4.2 g (0.020 mol) of 4-(4-fluoro-phenyl)-1,2,3,6-tetrahydropyridine hydrochloride and 8.0 g (0.060 mol) of dry potassium carbonate in 60 ml of dimethylformamide 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 recrystallized twice from ethyl acetate/cyclohexane and then from hot ethanol. 1.4 g (21%) of 5-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-propyl-pyrimidin-4-ylamine were obtained as white crystals; m.p. 142°-145°.

후처리

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

출처 및 근거

ORD 기록
ord-ae2c5862eac149559da4265b4b9144dc
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05688798

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