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

HRID 2108145

反応式

HRID 2108145 の反応式
[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

参加物

5

反応物 2

HCID 4090619(2,4-Dinitrophenyl)(4-methylpiperazin-1-yl)methanoneHCID 178418361HCID 178418361、化合物2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6b5d93b508194501913dbc973e496227
出典データセット
uspto-grants-1990_06
特許番号
US04937306

関連ノート

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