Methanol → HCID 11101016, 화합물

HRID 612138노트

반응식

HRID 612138 반응식
[Br:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:22][CH2:23][CH3:24])=[C:16]([N+:19]([O-])=O)[CH:17]=3)[N:12]=[CH:11][C:10]=2[C:25]#[N:26])[CH:5]=[CH:6][CH:7]=1.[Cl-].[NH4+].CO>O.C(OCC)(=O)C.[Fe]>[NH2:19][C:16]1[CH:17]=[C:18]2[C:13](=[CH:14][C:15]=1[O:22][CH2:23][CH3:24])[N:12]=[CH:11][C:10]([C:25]#[N:26])=[C:9]2[NH:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Br:1])[CH:3]=1

참가 물질

7

반응물 3

HCID 887MethanolHCID 25517Ammonium ChlorideHCID 11144112HCID 11144112, 화합물

생성물 1

HCID 11101016HCID 11101016, 화합물

시약·촉매·용매 3

HCID 23925Iron촉매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 2.5 g (6 mmol) of 4-[(3-bromophenyl)amino]-7-ethoxy-6-nitro-quinoline-3-carbonitrile, 2.4 g (45 mmol) of ammonium chloride, and 1.5 g (27 mmol) iron was stirred at reflux in 40 ml of water and 40 ml of methanol for 4 hours. The mixture was diluted with 500 ml of hot ethyl acetate and the hot mixture was filtered. The filtration was washed with saturated sodium chloride solution and then the organic layer was dried over sodium sulfate. The solution was concentrated and 1.5 of beige solid was collected: mass spectrum (electrospray, m/e): M+H 382.8 and 384.8.

후처리

  1. filtrationthe hot mixture was filtered
  2. filtrationThe filtration
  3. washwas washed with saturated sodium chloride solution
  4. dry with materialthe organic layer was dried over sodium sulfate
  5. concentrationThe solution was concentrated
  6. custom1.5 of beige solid was collected

출처 및 근거

ORD 기록
ord-10c386e382f54febbd4e582798b4b112
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06002008

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