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Dimethylformamide → 3-[2-(3-Methoxy-pyrrolidin-1-yl)-6-trifluoromethyl-pyridin-3-yl]-acrylic acid

HRID 2266004
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반응식

HRID 2266004 반응식
Cl[C:2]1[C:7]([CH:8]=[CH:9][C:10]([OH:12])=[O:11])=[CH:6][CH:5]=[C:4]([C:13]([F:16])([F:15])[F:14])[N:3]=1.[CH3:17][O:18][CH:19]1[CH2:23][CH2:22][NH:21][CH2:20]1.CN(C=O)C>CCOC(C)=O>[CH3:17][O:18][CH:19]1[CH2:23][CH2:22][N:21]([C:2]2[C:7]([CH:8]=[CH:9][C:10]([OH:12])=[O:11])=[CH:6][CH:5]=[C:4]([C:13]([F:16])([F:15])[F:14])[N:3]=2)[CH2:20]1
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참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 113554473-MethoxypyrrolidineHCID 723356323-(2-Chloro-6-trifluoromethyl-pyridin-3-yl)-acrylic acid

생성물 1

HCID 687825783-[2-(3-Methoxy-pyrrolidin-1-yl)-6-trifluoromethyl-pyridin-3-yl]-acrylic acid수율 98%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of 3-(2-chloro-6-trifluoromethyl-pyridin-3-yl)-acrylic acid (50 mg, 0.198 mmol) in 3-methoxy-pyrrolidine (40 mg, 0.396 mmol) was added DMF (1.0 ml). The mixture was stirred for 12 hours at room temperature. The reaction mixture was diluted with EtOAc and then washed two times with 1N-HCl and brine, dried over MgSO4, filtered and concentrated under reduced pressure. The crude residue was chromatographed to yield the 3-[2-(3-methoxy-pyrrolidin-1-yl)-6-trifluoromethyl-pyridin-3-yl]-acrylic acid (59 mg, 98%).

후처리

  1. washwashed two times with 1N-HCl and brine
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude residue was chromatographed

출처 및 근거

ORD 기록
ord-7cdb31048bb84fca974a037774f49f65
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858621B2

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