alpha-Naphthyl isocyanate → N-(2-Hydroxy-4-nitrophenyl)-N′-1-naphthalenylurea

HRID 1956637노트

반응식

HRID 1956637 반응식
[OH:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:3]=1[NH2:4].[C:12]1([N:22]=[C:23]=[O:24])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:14][CH:13]=1>>[OH:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:3]=1[NH:4][C:23]([NH:22][C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:14][CH:13]=1)=[O:24]

참가 물질

3

반응물 2

HCID 66589alpha-Naphthyl isocyanateHCID 49847212-Amino-5-Nitrophenol

생성물 1

HCID 21184716N-(2-Hydroxy-4-nitrophenyl)-N′-1-naphthalenylurea

실험 절차

N-(2-Hydroxy-4-nitrophenyl)-N'-(1-naphthyl)urea was prepared from 2-hydroxy 4-nitro aniline (500 mg, 3.24 mmol) and 1-naphthyl isocyanate (3.24 mmol) according to the procedure in General Method B. The product precipitated from methylene chloride and filtered. The resulting solid was titruated with 1:3 triethyl amine:methylene chloride. The filterate was concentrated in vacuo. The resulting residue was dissolved in methylene chloride and treated with 1N HCl in water. The desired product precipitated from solution and was collected by filtration(0.11 g, 10%). EI-MS m/z 324(M+H)+

후처리

  1. customThe product precipitated from methylene chloride
  2. filtrationfiltered
  3. concentrationThe filterate was concentrated in vacuo
  4. dissolutionThe resulting residue was dissolved in methylene chloride
  5. additiontreated with 1N HCl in water
  6. customThe desired product precipitated from solution
  7. filtrationwas collected by filtration(0.11 g, 10%)

출처 및 근거

ORD 기록
ord-06cd8e8db5294396955fab612c36d3b9
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05780483

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