[1-(2-Azidoethyl)-2-(phenylmethylene)hydrazino]oxoacetic acid, ethyl ester → 1-(Benzylideneamino)piperazine-2,3-dione

HRID 1449140

反応式

HRID 1449140 の反応式
[N:1]([CH2:4][CH2:5][N:6]([C:15](=[O:21])[C:16](OCC)=[O:17])[N:7]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[N+]=[N-].[H][H]>[Pd].CC([O-])=O.CC([O-])=O.[Pb+2].C(O)C>[C:9]1([CH:8]=[N:7][N:6]2[CH2:5][CH2:4][NH:1][C:16](=[O:17])[C:15]2=[O:21])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

5

反応物 2

HCID 86736838[1-(2-Azidoethyl)-2-(phenylmethylene)hydrazino]oxoacetic acid, ethyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 538480401-(Benzylideneamino)piperazine-2,3-dione

試薬・触媒・溶媒 2

HCID 131709914Lindlars catalyst触媒HCID 702Ethanol溶媒

実験手順

2 g. of the ethyl ester product from part (d) are dissolved in 100 ml. of ethanol. 0.5 g. of Lindlar catalyst are added and the reaction mixture is stirred for four hours at room temperature under two atmospheres of hydrogen. At intervals the reaction mixture is filtered. After completion of the slow absorption of hydrogen, the reaction solution is flooded with nitrogen and then heated to a boil. This mixture is filtered while hot and after cooling 1 g. of crude product is obtained from the filtrate. Recrystallization from water yields as white crystals purified 1-[(phenylmethylene)amino]-2,3-piperazinedione; m.p. 229°-231°.

後処理

  1. filtrationAt intervals the reaction mixture is filtered
  2. customAfter completion of the slow absorption of hydrogen
  3. temperatureheated to a boil
  4. filtrationThis mixture is filtered while hot and
  5. temperatureafter cooling 1 g
  6. customof crude product is obtained from the filtrate
  7. customRecrystallization from water
  8. customyields as white crystals
  9. custompurified 1-[(phenylmethylene)amino]-2,3-piperazinedione

出典と根拠

ORDレコード
ord-d718b6b4670e41c6b38b873d2d4d162e
出典データセット
uspto-grants-1980_02
特許番号
US04189482

関連ノート

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