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

HRID 851782

반응식

HRID 851782 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 131709914Lindlars catalyst촉매HCID 702Ethanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-bf4ee007285d4286a35da233d27efc0f
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04386199

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