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Cyclopropylamine → CID 74043826

HRID 232658
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HRID 232658 반응식
[CH3:1][C:2]1[C:7]([C:8]([C:10](=[CH:16]OCC)[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[O:9])=[C:6]([F:20])[C:5]([F:21])=[C:4]([F:22])[C:3]=1[F:23].[CH:24]1([NH2:27])[CH2:26][CH2:25]1>C(O)C>[CH3:1][C:2]1[C:7]([C:8]([C:10](=[CH:16][NH:27][CH:24]2[CH2:26][CH2:25]2)[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[O:9])=[C:6]([F:20])[C:5]([F:21])=[C:4]([F:22])[C:3]=1[F:23]
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참가 물질

4

반응물 2

HCID 69828CyclopropylamineHCID 54293321Ethyl 2-(2-methyl-3,4,5,6-tetrafluorobenzoyl)3-ethoxyacrylate

생성물 1

HCID 178471859CID 74043826수율 91.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl 2-(6-methyl-2,3,4,5-tetrafluorobenzoyl)-3-ethoxyacrylate (5 g) is dissolved in ethanol (25 ml) and thereto cyclopropylamine (1.0 g) is added dropwise under ice-cooling. After stirring at room temperature for 30 minutes, the mixture is concentrated and the residue is purified with column chromatography (silica-gel, dichloromethane: n-hexane =1:1) to give ethyl 2-(6-methyl-2,3,4,5-tetrafluorobenzoyl)-3-cyclopropylaminoacrylate (4.74 g), as white plates, m.p. 78°-79° C. (recrystallized from petroleum ether-n-hexane).

후처리

  1. temperaturecooling
  2. concentrationthe mixture is concentrated
  3. customthe residue is purified with column chromatography (silica-gel, dichloromethane: n-hexane =1:1)

출처 및 근거

ORD 기록
ord-c5771fb30d7b47639eb92cad57aca216
출처 데이터셋
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05591744

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