Diethyl Oxalate → HCID 68631253、化合物

HRID 1855471ノート

反応式

HRID 1855471 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 68631253HCID 68631253、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-316803638d2a4065bcf714925f59f872
出典データセット
uspto-grants-2015_02
特許番号
US08962834B2

反応ノート

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