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O-(2,2,2-Trifluoroethyl)hydroxylamine hydrochloride → 6-[(E)-3-[3-[(Z)-C-methyl-N-(2,2,2-trifluoroethoxy)carbonimidoyl]azetidin-1-yl]-3-oxoprop-1-enyl]-3,4-dihydro-1H-1,8-naphthyridin-2-one

HRID 83056
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HRID 83056 반응식
Cl.[F:2][C:3]([F:8])([F:7])[CH2:4][O:5][NH2:6].[C:9]([CH:12]1[CH2:15][N:14]([C:16](=[O:30])/[CH:17]=[CH:18]/[C:19]2[CH:20]=[C:21]3[C:26](=[N:27][CH:28]=2)[NH:25][C:24](=[O:29])[CH2:23][CH2:22]3)[CH2:13]1)(=O)[CH3:10]>CO>[O:30]=[C:16]([N:14]1[CH2:15][CH:12](/[C:9](=[N:6]\[O:5][CH2:4][C:3]([F:8])([F:7])[F:2])/[CH3:10])[CH2:13]1)/[CH:17]=[CH:18]/[C:19]1[CH:20]=[C:21]2[C:26](=[N:27][CH:28]=1)[NH:25][C:24](=[O:29])[CH2:23][CH2:22]2
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참가 물질

4

반응물 2

HCID 19853822O-(2,2,2-Trifluoroethyl)hydroxylamine hydrochlorideHCID 67154676(E)-6-(3-(3-acetylazetidin-1-yl)-3-oxoprop-1-enyl)-3,4-dihydro-1,8-naphthyridin-2(1H)-one

생성물 1

HCID 529507506-[(E)-3-[3-[(Z)-C-methyl-N-(2,2,2-trifluoroethoxy)carbonimidoyl]azetidin-1-yl]-3-oxoprop-1-enyl]-3,4-dihydro-1H-1,8-naphthyridin-2-one수율 74.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2,2,2-Trifluoroethoxyamine hydrochloride (37 mg, 0.24 mmol) was added to a solution of (E)-6-(3-(3-acetylazetidin-1-yl)-3-oxoprop-1-enyl)-3,4-dihydro-1,8-naphthyridin-2(1H)-one (50 mg, 0.16 mmol) in methanol (4 mL). The reaction mixture was stirred at room temperature for 3 hours. After concentration to dryness the residue was diluted by addition of dichloromethane (50 mL) and saturated sodium bicarbonate solution (10 mL). The aqueous phase was extracted with dichloromethane (2×40 mL). The combined organic phases were washed with a saturated solution of sodium chloride (1×20 mL), dried over sodium sulfate, filtered and concentrated to dryness. The residue was purified by chromatography on silica gel using ethyl acetate/methanol (95:5) as eluent to obtain the title product as a white solid (47 mg, 50%).

후처리

  1. concentrationAfter concentration to dryness the residue
  2. additionwas diluted by addition of dichloromethane (50 mL) and saturated sodium bicarbonate solution (10 mL)
  3. extractionThe aqueous phase was extracted with dichloromethane (2×40 mL)
  4. washThe combined organic phases were washed with a saturated solution of sodium chloride (1×20 mL)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness
  8. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-9755dfe6fdc947ddaa5ce9c38564f4a0
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846711B2

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