Benzene → Diethyl[(6-amino-4-quinazolinylamino)methylene]propanedioate

HRID 354880ノート

反応式

HRID 354880 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[CH:9][N:8]=[C:7]2[NH:14][CH:15]=[C:16]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:17]([O:19][CH2:20][CH3:21])=[O:18])([O-])=O.C1C=CC=CC=1>CN(C)C=O.[Pd].[H][H]>[NH2:1][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[CH:9][N:8]=[C:7]2[NH:14][CH:15]=[C:16]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:17]([O:19][CH2:20][CH3:21])=[O:18]

参加物

6

反応物 2

HCID 241BenzeneHCID 13060485Diethyl[(6-nitro-4-quinazolinylamino)methylene]propanedioate

生成物 1

HCID 20266113Diethyl[(6-amino-4-quinazolinylamino)methylene]propanedioate

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 6228Dimethylformamide溶媒HCID 178418361HCID 178418361、化合物溶媒

実験手順

A solution of diethyl [(6-nitro-4-quinazolinylamino)methylene]propanedioate (10.8 g) in N,N-dimethylformamide (325 ml) was shaken with 10% palladium on carbon (3.6 g) in hydrogen atmosphere at ambient temperature. After the absorption of hydrogen was finished, the catalyst was removed by filtration. The filtrate was concentrated under reduced pressure to give a residue, to which was added benzene. The mixture was concentrated under reduced pressure to give crude crystals of diethyl [(6-amino-4-quinazolinylamino)methylene]propanedioate.

後処理

  1. customAfter the absorption of hydrogen
  2. customthe catalyst was removed by filtration
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customto give a residue
  5. concentrationThe mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-960f093331be411d83f20829bb707eeb
出典データセット
uspto-grants-1983_03
特許番号
US04377580

反応ノート

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