Triethylamine → 5-[4-(4-Chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine

HRID 2294034ノート

反応式

HRID 2294034 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(N(CC)CC)C.Br.Br.Br[CH2:24][C:25]1[C:26]([NH2:32])=[N:27][C:28]([NH2:31])=[N:29][CH:30]=1>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:24][C:25]3[C:26]([NH2:32])=[N:27][C:28]([NH2:31])=[N:29][CH:30]=3)[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 974781-(4-Chlorophenyl)piperazineHCID 214736085-(Bromomethyl)pyrimidine-2,4-diamine dihydrobromide

生成物 1

HCID 214736515-[4-(4-Chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine収率 41.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 0.97 g (0.00493 mol) of 1-(4-chloro-phenyl)-piperazine in 35 ml of dimethylformamide was treated with 1.37 ml (0.00986 mol) of triethylamine and 0.60 g (0.0016 mol) of 5-bromomethyl-pyrimidine-2,4-diamine dihydrobromide and the mixture was stirred at room temperature under argon for 60 hours. The mixture was completely freed from the solvents. The residue was chromatographed over silica gel with acetonitrile/methanol 1:1 as the eluent, digested in dichloromethane/water 1:1 and subsequently filtered off under suction. 0.21 g (40%) of 5-[4-(4-chloro-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine was obtained as white crystals; m.p. 296°-298°.

後処理

  1. customThe residue was chromatographed over silica gel with acetonitrile/methanol 1:1 as the eluent
  2. filtrationsubsequently filtered off under suction

出典と根拠

ORDレコード
ord-26c0f29b4074491eb14161b23fbd5073
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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