Pyridine → 1-(5-Methyl-4-phenyl-4H-1,2,4-triazol-3-yl)piperazine

HRID 1720762노트

반응식

HRID 1720762 반응식
Br[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:5]([CH3:13])=[N:4][N:3]=1.[NH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.N1C=CC=CC=1>CO.C(Cl)Cl>[CH3:13][C:5]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:2]([N:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)=[N:3][N:4]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 4837PiperazineHCID 12217059HCID 12217059, 화합물

생성물 1

HCID 224187621-(5-Methyl-4-phenyl-4H-1,2,4-triazol-3-yl)piperazine

시약·촉매·용매 1

HCID 21226129Dichloromethane methanol용매

실험 절차

A mixture of 3-bromo-5-methyl-4-phenyl-4H-1,2,4-triazole (4.16 g), 15.07 g of piperazine and 20 ml of pyridine is stirred at 100° under nitrogen for 22 h. The reaction is monitored by TLC (8% methanol/methylene chloride) and after this period of time no change occurs. The mixture is subsequently placed in a Parr bomb and heated in an oil bath at 180° for 24 h. Bomb pressure increases by 40 psi. The mixture is worked up by partitioning between chloroform and water. The organic phase is washed with saturated aqueous sodium bicarbonate (2×) and with saline (2×), dried over sodium sulfate and concentrated to a solid, the product is recrystallized in ethyl acetate, MS [M+H]+ 243.1484

후처리

  1. temperatureheated in an oil bath at 180° for 24 h
  2. temperatureincreases by 40 psi
  3. customby partitioning between chloroform and water
  4. washThe organic phase is washed with saturated aqueous sodium bicarbonate (2×) and with saline (2×)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated to a solid
  7. customthe product is recrystallized in ethyl acetate

출처 및 근거

ORD 기록
ord-170b2d12565145f5a11c9ef827bea9b7
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05506354

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