Water → HCID 57387083, 화합물

HRID 1800569노트

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HRID 1800569 반응식
[Cl:1][C:2]1[C:27]([C:28]2([C:31]#[N:32])[CH2:30][CH2:29]2)=[CH:26][CH:25]=[CH:24][C:3]=1[C:4]([NH:6][C:7]1[CH:12]=[C:11]([O:13][C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-])=O)=[CH:16][N:15]=2)[CH:10]=[CH:9][C:8]=1[F:23])=[O:5].[Cl-].[Ca+2].[Cl-].O.[OH-].[Na+]>C(O)C.[Fe].C(OCC)(=O)C>[NH2:20][C:17]1[CH:18]=[CH:19][C:14]([O:13][C:11]2[CH:10]=[CH:9][C:8]([F:23])=[C:7]([NH:6][C:4](=[O:5])[C:3]3[CH:24]=[CH:25][CH:26]=[C:27]([C:28]4([C:31]#[N:32])[CH2:29][CH2:30]4)[C:2]=3[Cl:1])[CH:12]=2)=[N:15][CH:16]=1

참가 물질

8

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 5284359Calcium ChlorideHCID 573842802-chloro-3-(1-cyanocyclopropyl)-N-{2-fluoro-5-[(5-nitropyridin-2-yl)oxy]phenyl}benzamide

생성물 1

HCID 57387083HCID 57387083, 화합물수율 69%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

A suspension of 2-chloro-3-(1-cyanocyclopropyl)-N-{2-fluoro-5-[(5-nitropyridin-2-yl)oxy]phenyl}benzamide (6.60 g, 14.6 mmol), iron powder (1.68 g, 30 mmol) and calcium chloride (3.33 g, 30 mmol) in ethanol (80 mL)-water (20 mL) was stirred at 80° C. overnight. The reaction mixture was poured into 0.5N aqueous sodium hydroxide solution (500 mL), ethyl acetate (300 mL) was added, the mixture was stirred, and the insoluble material was filtered through celite. The ethyl acetate layer was separated from the filtrate, and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was triturated with diethyl ether to give the title compound (4.23 g, 69%) as a pale-yellow amorphous.

후처리

  1. additionwas added
  2. stirringthe mixture was stirred
  3. filtrationthe insoluble material was filtered through celite
  4. customThe ethyl acetate layer was separated from the filtrate
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationThe insoluble material was filtered off
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe obtained residue was triturated with diethyl ether

출처 및 근거

ORD 기록
ord-8f8f8ac45b224908b8b415921d128e73
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08344135B2

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