Diethyl Oxalate → HCID 68631253, 화합물

HRID 1855471

반응식

HRID 1855471 반응식
CC(C)([O-])C.[K+].[F:7][C:8]1[CH:9]=[C:10]([C:16](=[O:18])[CH3:17])[CH:11]=[C:12]([F:15])[C:13]=1[F:14].[C:19](OCC)(=[O:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21]>C(OCC)C>[O:25]=[C:19]([CH2:17][C:16](=[O:18])[C:10]1[CH:9]=[C:8]([F:7])[C:13]([F:14])=[C:12]([F:15])[CH:11]=1)[C:20]([O:22][CH2:23][CH3:24])=[O:21]

참가 물질

5

반응물 3

HCID 7268Diethyl OxalateHCID 27769073',4',5'-TrifluoroacetophenoneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 68631253HCID 68631253, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
0 °C

실험 절차

Potassium tert.-butoxide (1.12 g, 10.0 mmol) was added to a solution of 1-(3,4,5-trifluoro-phenyl)-ethanone (1.74 g, 10.0 mmol) and diethyl oxalate (1.49 mL, 11.0 mmol) in diethyl ether (20 mL) cooled to 0° C. The heterogenous mixture was stirred for 15 min at 0° C. followed by 15 h at 20° C. The mixture was partitioned between 3 N hydrochloric acid (20 mL) and diethyl ether (50 mL). The organic layer was washed with brine (20 mL), dried over sodium sulfate and evaporated under reduced pressure and the residual oil was crystallized from diethyl ether/heptane to give the title compound as a white solid.

후처리

  1. waitfollowed by 15 h at 20° C
  2. customThe mixture was partitioned between 3 N hydrochloric acid (20 mL) and diethyl ether (50 mL)
  3. washThe organic layer was washed with brine (20 mL)
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure
  6. customthe residual oil was crystallized from diethyl ether/heptane

출처 및 근거

ORD 기록
ord-316803638d2a4065bcf714925f59f872
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962834B2

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