(2,4-Dinitrophenyl)(4-methylpiperazin-1-yl)methanone → N1-methyl-N4-(2,4-diaminobenzoyl)-piperazine

HRID 1087169

반응식

HRID 1087169 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8](=[O:21])[C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[CH:11][C:10]=2[N+:18]([O-])=O)[CH2:4][CH2:3]1.[H][H]>[Pd].CO>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8](=[O:21])[C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][C:10]=2[NH2:18])[CH2:4][CH2:3]1

참가 물질

5

반응물 2

HCID 4090619(2,4-Dinitrophenyl)(4-methylpiperazin-1-yl)methanoneHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 54115179N1-methyl-N4-(2,4-diaminobenzoyl)-piperazine수율 85.7%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A 2 liter autoclave was charged with 148 g of N1 -methyl-N4 -(2,4-dinitrobenzoyl)piperazine, 1300 ml of methanol and 5 g of a 5% palladium on carbon/50% water catalyst. The mixture was hydrogenated under 800 psi hydrogen pressure while maintaining the temperature below 100° C. with cooling. Hydrogen uptake ceased after 30 min. The mixture was cooled, filtered and the methanol removed under reduced pressure to give 101 g of N1 -methyl-N4 -(2,4-diaminobenzoyl)- piperazine, a light tan solid, mp 192° C.

후처리

  1. temperaturewhile maintaining the temperature below 100° C.
  2. temperaturewith cooling
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. customthe methanol removed under reduced pressure

출처 및 근거

ORD 기록
ord-b3fa88c30fc1498d809457609fe764ca
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034426

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