Triethylamine → 2-Methyl-5-[4-(2-nitro-phenyl)-piperazin-1-ylmethyl]-pyrimidin-4-ylamine

HRID 2294002

反応式

HRID 2294002 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)([O-:3])=[O:2].C(N(CC)CC)C.Cl.Cl[CH2:25][C:26]1[C:27]([NH2:33])=[N:28][C:29]([CH3:32])=[N:30][CH:31]=1>CN(C)C=O>[CH3:32][C:29]1[N:28]=[C:27]([NH2:33])[C:26]([CH2:25][N:13]2[CH2:12][CH2:11][N:10]([C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[N+:1]([O-:3])=[O:2])[CH2:15][CH2:14]2)=[CH:31][N:30]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1009491-(2-Nitrophenyl)piperazineHCID 214736115-(Chloromethyl)-2-methylpyrimidin-4-amine--hydrogen chloride (1/1)

生成物 1

HCID 214736622-Methyl-5-[4-(2-nitro-phenyl)-piperazin-1-ylmethyl]-pyrimidin-4-ylamine収率 76.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 1.25 g (0.0060 mol) of 1-(2-nitro-phenyl)-piperazine and 2.1 ml (0.015 mol) of triethylamine in 20 ml of dimethylformamide was treated with 0.97 g (0.0050 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride and the mixture was stirred at room temperature under argon for 3 hours. The mixture was completely freed from the solvents and the residue was triturated in 20 ml of water. The resulting crystals were filtered off under suction, dried and chromatographed over silica gel with dichloromethane/methanol 19:1 as the eluent. 1.25 g (76%) of 2-methyl-5- [4-(2-nitro-phenyl )-piperazin-1-ylmethyl]-pyrimidin-4-ylamine were obtained as a yellow solid.

後処理

  1. customthe residue was triturated in 20 ml of water
  2. filtrationThe resulting crystals were filtered off under suction
  3. customdried
  4. customchromatographed over silica gel with dichloromethane/methanol 19:1 as the eluent

出典と根拠

ORDレコード
ord-fa14a891f71440eda38d04d4f8f6b9a3
出典データセット
uspto-grants-1997_11
特許番号
US05688798

関連ノート

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