Hydrochloric Acid → HCID 67037009、化合物

HRID 1401295ノート

反応式

HRID 1401295 の反応式
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][C:6]([C:8]1[C:9]([C:15]([F:18])([F:17])[F:16])=[N+:10]([O-:14])[CH:11]=[CH:12][CH:13]=1)=[O:7])[CH3:2].Br[CH2:21][C:22]([C:24]1[CH:29]=[C:28]([N+:30]([O-:32])=[O:31])[C:27]([O:33][CH3:34])=[C:26]([O:35][CH3:36])[CH:25]=1)=O.Cl>N1C=CC=CC=1>[CH3:36][O:35][C:26]1[CH:25]=[C:24]([C:22]2[C:5]([C:4]([O:3][CH2:1][CH3:2])=[O:19])=[C:6]([C:8]3[C:9]([C:15]([F:17])([F:16])[F:18])=[N+:10]([O-:14])[CH:11]=[CH:12][CH:13]=3)[O:7][CH:21]=2)[CH:29]=[C:28]([N+:30]([O-:32])=[O:31])[C:27]=1[O:33][CH3:34]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 67036724HCID 67036724、化合物HCID 714457912-Bromo-1-(3,4-dimethoxy-5-nitrophenyl)ethanone

生成物 1

HCID 67037009HCID 67037009、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
70 °C

実験手順

To a stirred solution of 3-(3-ethoxy-3-oxopropanoyl)-2-(trifluoromethyl)pyridine-1-oxide (1.39 g, 5 mmol) in pyridine (25 mL) was added 2-bromo-1-(3,4-dimethoxy-5-nitrophenyl)ethanone (1.67 g, 5.5 mmol). The reaction mixture was heated to 70° C. and stirred for 5 hours, then cooled to room temperature and poured onto 6 N aqueous HCl (100 mL). The precipitate was filtered off, washed with water and dried over P2O5 under vacuum. The solid was recrystallised from dichloromethane/isopropanol to give crude 3-(4-(3,4-dimethoxy-5-nitrophenyl)-3-(ethoxycarbonyl)furan-2-yl)-2-(trifluoromethyl)pyridine 1-oxide, 1.05 g (43%).

後処理

  1. temperaturecooled to room temperature
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. dry with materialdried over P2O5 under vacuum
  5. customThe solid was recrystallised from dichloromethane/isopropanol

出典と根拠

ORDレコード
ord-98cdad04dc5d479888bde889ebdff250
出典データセット
uspto-grants-2014_12
特許番号
US08907099B2

反応ノート

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