Hydrochloric Acid → HCID 20163296、化合物

HRID 246895ノート

反応式

HRID 246895 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1([C:16](=[O:19])[CH2:17][CH3:18])[CH:13]([CH3:14])[CH2:12][C:11]([CH3:15])=[CH:10][CH2:9]1.[H][H].Cl>C(OCC)C.O>[CH3:7][C:8]1([CH:16]([OH:19])[CH2:17][CH3:18])[CH:13]([CH3:14])[CH2:12][C:11]([CH3:15])=[CH:10][CH2:9]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 20163298HCID 20163298、化合物HCID 21226445Aluminium lithium hydrideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 20163296HCID 20163296、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

A solution of 0.075 moles (2.85 g) lithium aluminum hydride in 150 ml absolute diethyl ether was put in a 250-ml 3-necked flask with a magnetic stirrer, high-power condenser, dropping funnel and internal thermometer. 0.2 moles (36 g) 1-(1,4,6-trimethylcyclohex-3-en-1-yl)propan-1-one (as per Example 4) was added dropwise to this solution with cooling. Then heating with refluxing was carried out for an hour, followed by cooling, and water was added to the reaction mixture until hydrogen evolution ended. Then enough 2N hydrochloric acid was added so that the precipitate formed could be dissolved. Lastly the phases were separated, the organic phase dried with sodium sulfate and the solvent drawn off. After fractional distillation via a 30-cm Vigreux column the desired end product was obtained in practically quantitative yield.

後処理

  1. temperaturewith cooling
  2. temperatureThen heating
  3. temperaturewith refluxing
  4. waitwas carried out for an hour
  5. temperatureby cooling
  6. customformed could
  7. dissolutionbe dissolved
  8. customLastly the phases were separated
  9. dry with materialthe organic phase dried with sodium sulfate
  10. distillationAfter fractional distillation via a 30-cm Vigreux column the desired end product
  11. customwas obtained in practically quantitative yield

出典と根拠

ORDレコード
ord-23421fa86b8b46e2857c001b7d8da4ea
出典データセット
uspto-grants-1987_11
特許番号
US04704477

反応ノート

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