Hydrochloric Acid → HCID 67037009, 화합물

HRID 1401295노트

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HRID 1401295 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 67037009HCID 67037009, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
70 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-98cdad04dc5d479888bde889ebdff250
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08907099B2

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