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Ethyl Acetate → HCID 178487875, 화합물

HRID 1422973
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HRID 1422973 반응식
[C:1]([O:5][C:6](=[O:17])[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][CH:15]=[O:16])[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[Cl:18][C:19]1[CH:20]=[N:21][C:22]2[C:27]([C:28]=1[CH:29]=[O:30])=[N:26][C:25]([O:31][CH3:32])=[CH:24][CH:23]=2.N1CCC[C@H]1C(O)=O.C(OCC)(=O)C>CS(C)=O.O>[C:1]([O:5][C:6](=[O:17])[NH:7][C@H:8]1[CH2:9][CH2:10][C@H:11]([CH:14]([CH:15]=[O:16])[CH:29]([C:28]2[C:27]3[C:22](=[CH:23][CH:24]=[C:25]([O:31][CH3:32])[N:26]=3)[N:21]=[CH:20][C:19]=2[Cl:18])[OH:30])[CH2:12][CH2:13]1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 145742L-ProlineHCID 866715503-Chloro-6-methoxy-[1,5]naphthyridine-4-carbaldehydeHCID 178453924HCID 178453924, 화합물

생성물 1

HCID 178487875HCID 178487875, 화합물수율 39%

시약·촉매·용매 2

HCID 679
Dimethyl Sulfoxide
용매
HCID 962Water용매

실험 절차

A solution of [trans-4-(2-oxo-ethyl)-cyclohexyl]-carbamic acid tert-butyl ester (3.1 g, 25.1 mmol, 1.0 eq), 3-chloro-6-methoxy-[1,5]naphthyridine-4-carbaldehyde (5.6 g, 25.1 mmol, 1.0 eq) and L-proline (1.16 mg, 10.1 mmol, 0.4 eq) in dimethyl sulfoxide (100 mL) and water (15 mL) is stirred at room temperature for 16 hours. The reaction mixture is then extracted with ethyl acetate (500 mL) and water (500 mL). The organic layer is washed with brine (300 mL), dried over magnesium sulfate, filtered and concentrated to give a residue that is purified by column chromatography (silica gel, eluent: ethyl acetate:petroleum ether, 1:1, v/v) to afford {trans-4-[2-(3-chloro-6-methoxy-[1,5]naphthyridin-4-yl)-1-formyl-2-hydroxy-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester as a light yellow solid (4.5 g, 39% yield).

후처리

  1. extractionThe reaction mixture is then extracted with ethyl acetate (500 mL) and water (500 mL)
  2. washThe organic layer is washed with brine (300 mL)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give a residue that
  7. customis purified by column chromatography (silica gel, eluent

출처 및 근거

ORD 기록
ord-bd7928ae951b4003b0adba04bb4ecab1
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08927541B2

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