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

HRID 2294038ノート

反応式

HRID 2294038 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:5][CH:4]=1.C(N(CC)CC)C.Br.Br.Br[CH2:25][C:26]1[C:27]([NH2:33])=[N:28][C:29]([NH2:32])=[N:30][CH:31]=1>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH2:25][C:26]3[C:27]([NH2:33])=[N:28][C:29]([NH2:32])=[N:30][CH:31]=3)[CH2:11][CH2:10]2)=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2697221-(4-Methoxyphenyl)piperazineHCID 214736085-(Bromomethyl)pyrimidine-2,4-diamine dihydrobromide

生成物 1

HCID 214736195-[4-(4-Methoxy-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine収率 47%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 0.95 g (0.00494 mol) of 1-(4-methoxy-phenyl)-piperazine in 30 ml of dimethylformamide was treated with 1.37 ml (0.00986 mol) of triethylamine and 0.60 g (0.00164 mol) of 5-bromomethyl-pyrimidine-2,4-diamine dihydrobromide and the mixture was stirred at room temperature under argon for 65 hours. The mixture was completely freed from the solvents. The residue was chromatographed over silica gel with acetonitrile/methanol (1:1 ), digested in diethyl ether and subsequently filtered off under suction. 0.24 g (47%) of 5-[4-(4-methoxy-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine was obtained as white crystals; m.p. 239°-241°.

後処理

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

出典と根拠

ORDレコード
ord-c97c882a7aa249c09f11774b320d1579
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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