Methanol → 2-Amino-6-bromophenol

HRID 469804노트

반응식

HRID 469804 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:5]=1[OH:11])([O-])=O.CO>C1COCC1.[Ni]>[NH2:1][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:5]=1[OH:11]

참가 물질

5

반응물 2

HCID 887MethanolHCID 135454532-Bromo-6-nitrophenol

생성물 1

HCID 155315062-Amino-6-bromophenol

시약·촉매·용매 2

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매

실험 절차

5 g (22.9 mmol) 2-nitro-6-bromo-phenol (Fluka 67211) is hydrogenated in the presence of 0.1 g Ra—Ni (B113W EtOH, Degussa) in 100 ml of THF:MeOH=1:1. for 4 h. The reaction mixture is filtered (2 glass fiber filters used) and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, hexane:EtOAc=2:1) to afford the title compound as a reddish oil which slowly solidifies.

후처리

  1. filtrationThe reaction mixture is filtered (2 glass fiber filters used)
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe residue is purified by chromatography (silicagel, hexane:EtOAc=2:1)

출처 및 근거

ORD 기록
ord-991f4ad3cf6d4953aefaa3c986c6fd40
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629168B2

반응 노트

불러오는 중…