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Ethyl trifluoroacetate → HCID 17967065, 화합물

HRID 1767706
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HRID 1767706 반응식
[H-].[Na+].[CH3:3][S:4][C:5]1[CH:6]=[CH:7][C:8]([C:11](=[O:13])[CH3:12])=[N:9][CH:10]=1.[F:14][C:15]([F:22])([F:21])[C:16](OCC)=[O:17]>O1CCCC1>[F:14][C:15]([F:22])([F:21])[C:16](=[O:17])[CH2:12][C:11]([C:8]1[CH:7]=[CH:6][C:5]([S:4][CH3:3])=[CH:10][N:9]=1)=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 9794Ethyl trifluoroacetateHCID 24758Sodium hydrideHCID 200793671-(5-(Methylsulfanyl)pyridin-2-yl)ethan-1-one

생성물 1

HCID 17967065HCID 17967065, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A stirring solution of sodium hydride (0.253 g, 6.31 mmol) in anhydrous tetrahydrofuran (20 mL) was cooled under nitrogen to 0° C. before the addition of 1-(5-methylsulfanyl-pyridin-2-yl)-ethanone (0.880 g, 5.26 mmol) in anhydrous tetrahydrofuran (20 mL). Ethyl trifluoroacetate (0.751 mL, 6.31 mmol) was added dropwise and the reaction allowed to rise in temperature to 22° C., then heated to reflux and stirred under nitrogen for 17 hours. The solvent was removed and the residue partitioned between saturated aqueous ammonium chloride (10 mL) and dichloromethane (10 mL). The aqueous layer was separated and extracted with DCM (×3). The organic layers were combined, dried and the solvent removed to yield the title compound: MS m/z 264 (M+1).

후처리

  1. customto rise in temperature to 22° C.
  2. temperatureheated
  3. temperatureto reflux
  4. customThe solvent was removed
  5. customthe residue partitioned between saturated aqueous ammonium chloride (10 mL) and dichloromethane (10 mL)
  6. customThe aqueous layer was separated
  7. extractionextracted with DCM (×3)
  8. customdried
  9. customthe solvent removed

출처 및 근거

ORD 기록
ord-4778132dfcb84a13844ce6b9088f24dc
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07235560B2

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