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

HRID 354880노트

반응식

HRID 354880 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 6228Dimethylformamide용매HCID 178418361HCID 178418361, 화합물용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-960f093331be411d83f20829bb707eeb
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04377580

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