Methanol → HCID 11101016、化合物

HRID 1935055ノート

反応式

HRID 1935055 の反応式
[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

参加物

7

反応物 3

HCID 887MethanolHCID 25517Ammonium ChlorideHCID 11144112HCID 11144112、化合物

生成物 1

HCID 11101016HCID 11101016、化合物

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1299012111ed423cba5ed5d6ed372762
出典データセット
uspto-grants-2002_05
特許番号
US06384051B1

反応ノート

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