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

HRID 2294002

반응식

HRID 2294002 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa14a891f71440eda38d04d4f8f6b9a3
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05688798

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