Hydrochloric Acid → 2-Octanone, 1,1,1-trifluoro-

HRID 2073421ノート

反応式

HRID 2073421 の反応式
[Mg].[CH2:2](Br)[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[F:9][C:10]([F:15])([F:14])[C:11](O)=[O:12].Cl>CCOCC>[F:9][C:10]([F:15])([F:14])[C:11](=[O:12])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 81011-BromohexaneHCID 5462224Magnesium

生成物 1

HCID 959112-Octanone, 1,1,1-trifluoro-収率 54%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒3 回

実験手順

In a nitrogen atmosphere, 9.12 g (380 mM) of magnesium into 120 ml of ether, and 59.4 g (360 mM) of hexyl bromide dissolved in 30 ml of ether was added thereto, followed by 1.5 hours of heat refluxing. After cooling by standing and with ice, 13.68 g (120 mM) of trifluoroacetic acid dissolved in 30 ml of ether was added. After being stirred for 7 hours under cooling with ice, the system was subjected to hydrolysis with addition of hydrochloric acid, followed by extraction with ether and drying of the resultant ether layer with anhydrous sodium sulfate. The dried product was distilled under normal pressure to obtain 11.8 g of 1,1,1-trifluoro-2-octanone. Yield: 46%.

後処理

  1. additionwas added
  2. temperatureof heat
  3. temperaturerefluxing
  4. temperatureAfter cooling
  5. additionwas added
  6. temperatureunder cooling with ice
  7. extractionfollowed by extraction with ether
  8. dry with materialdrying of the resultant ether layer with anhydrous sodium sulfate
  9. distillationThe dried product was distilled under normal pressure

出典と根拠

ORDレコード
ord-ccf0ce45b8d243fba9b886fc98cc8ecd
出典データセット
uspto-grants-1990_04
特許番号
US04917817

反応ノート

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