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Water → HCID 86626076, 화합물

HRID 390597
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HRID 390597 반응식
FC(F)(F)C(O)=O.C(OC([CH2:15][NH:16][C:17]1[CH:18]=[C:19]([C:23]2[N:28]=[CH:27][C:26](/[CH:29]=[C:30](\[O:36][CH2:37][CH3:38])/[C:31]([O:33][CH2:34][CH3:35])=[O:32])=[CH:25][CH:24]=2)[CH:20]=[CH:21][CH:22]=1)=O)(C)(C)C.O>ClCCl>[CH2:37]([O:36]/[C:30](=[CH:29]\[C:26]1[CH:27]=[N:28][C:23]([C:19]2[CH:20]=[CH:21][CH:22]=[C:17]([NH:16][CH3:15])[CH:18]=2)=[CH:24][CH:25]=1)/[C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH3:38]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 86626077HCID 86626077, 화합물

생성물 1

HCID 86626076HCID 86626076, 화합물수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

0.62 mL (7.0 mmol) of trifluoroacetic acid is added to a solution of 0.30 g (0.7 mmol) of ethyl (Z)-3-{6-[3-(tert-butoxycarbonylmethylamino)phenyl]pyrid-3-yl}-2-ethoxyacrylate in 10 mL of dichloromethane. The reaction mixture is stirred at room temperature for 20 hours. The reaction is stopped by addition of 10 mL of water and extraction with dichloromethane. The organic phases are combined and then dried over magnesium sulfate. After filtration, the solvents are evaporated off. The crude product obtained is purified by chromatography on a column of silica eluted with an 80/20 heptane/ethyl acetate mixture to give 0.19 g (86%) of ethyl (Z)-2-ethoxy-3-[6-(3-methylaminophenyl)pyrid-3-yl]acrylate in the form of a yellow solid.

후처리

  1. dry with materialdried over magnesium sulfate
  2. filtrationAfter filtration
  3. customthe solvents are evaporated off
  4. customThe crude product obtained
  5. customis purified by chromatography on a column of silica
  6. washeluted with an 80/20 heptane/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-0825cd0529a14d26a854428f368966ac
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383652B2

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