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

HRID 2294026ノート

反応式

HRID 2294026 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-0782c0c1511c480bbfd00c3685b66925
出典データセット
uspto-grants-1997_11
特許番号
US05688798

反応ノート

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