Triethylamine → 2-Methyl-5-(4-phenethyl-piperazin-1-ylmethyl)-pyrimidin-4-ylamine

HRID 2294026

반응식

HRID 2294026 반응식
Cl.Cl[CH2:3][C:4]1[C:5]([NH2:11])=[N:6][C:7]([CH3:10])=[N:8][CH:9]=1.[CH2:12]([N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(CC)CC)C>CN(C)C=O>[CH3:10][C:7]1[N:6]=[C:5]([NH2:11])[C:4]([CH2:3][N:23]2[CH2:24][CH2:25][N:20]([CH2:12][CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:21][CH2:22]2)=[CH:9][N:8]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 792141-PhenethylpiperazineHCID 214736115-(Chloromethyl)-2-methylpyrimidin-4-amine--hydrogen chloride (1/1)

생성물 1

HCID 214736142-Methyl-5-(4-phenethyl-piperazin-1-ylmethyl)-pyrimidin-4-ylamine수율 83%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 0.30 g (0.0019 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride in 20 ml of dimethylformamide was treated with 0.30 g (0.00157 mol) of 1-phenethyl-piperazine and 0.66 ml (0.0047 mol) of triethylamine and the mixture was stirred at room temperature under argon for 36 hours. The mixture was completely freed from the solvents. The residue was partitioned between dichloromethane and water, extracted, chromatographed over silica gel with methanol as the eluent and recrystallized from toluene. 0.39 g (83%) of 2-methyl-5-(4-phenethyl-piperazin-1-ylmethyl)-pyrimidin-4-ylamine was obtained as white crystals; m.p. 162°-165°.

후처리

  1. customThe residue was partitioned between dichloromethane and water
  2. extractionextracted
  3. customchromatographed over silica gel with methanol as the eluent
  4. customrecrystallized from toluene

출처 및 근거

ORD 기록
ord-0782c0c1511c480bbfd00c3685b66925
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05688798

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