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

HRID 1719940ノート

反応式

HRID 1719940 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.C1(C)C=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 1140TolueneHCID 13060485Diethyl[(6-nitro-4-quinazolinylamino)methylene]propanedioate

生成物 1

HCID 20266113Diethyl[(6-amino-4-quinazolinylamino)methylene]propanedioate収率 97.4%

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 suspension of diethyl [(6-nitro-4-quinazolinylamino)methylene]propanedioate (2.8 g) in N,N-dimethylformamide (152 ml) was shaken with 10% palladium on carbon (0.93 g) in hydrogen atmosphere at ambient temperature for an hour. After the reaction was completed, the catalyst was removed by filtration and washed with chloroform. The combined filtrate and washing was concentrated under reduced pressure to give a residue, to which was added toluene and concentrated under reduced pressure. This operation was repeated to give crystalline diethyl [(6-amino-4-quinazolinylamino)methylene]propanedioate (2.50 g).

後処理

  1. customthe catalyst was removed by filtration
  2. washwashed with chloroform
  3. washThe combined filtrate and washing
  4. concentrationwas concentrated under reduced pressure
  5. customto give a residue
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-75e9ac969c9646b4b84c07b958786e63
出典データセット
uspto-grants-1985_09
特許番号
US04543356

反応ノート

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