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Hydrochloric Acid → HCID 11321150、化合物

HRID 1655764
ノート
印刷プレビュー

反応式

HRID 1655764 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C@H:13]([CH:17]([CH3:19])[CH3:18])[C:14](O)=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl>CCOCC>[C:7]1([C@H:13]([CH:17]([CH3:19])[CH3:18])[CH2:14][OH:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7233172(S)-3-methyl-2-phenylbutanoic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 11321150HCID 11321150、化合物収率 105.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A suspension of 19.5, g (0.51 mol) of lithium aluminium hydride in 750 ml of absolute ether was heated to reflux. Within 4 hours there was added, dropwise, a solution of 54.5 g (0.307 mol) of (S)-(+)-2-phenyl 3-methylbutyric acid in 250 ml of absolute ether. After heating to reflux for a further 2 hours, the suspension was treated carefully with 1N hydrochloric acid and the ether phase was washed with water, dilute sodium bicarbonate solution, and once more with water. After drying the organic phase over sodium sulfate and evaporation under reduced pressure, there were obtained 53.1 g of (S)-(+)-2-phenyl-3-methylbutanol as a thick oil which was used directly in the next step.

後処理

  1. temperaturewas heated to reflux
  2. additionWithin 4 hours there was added
  3. temperatureAfter heating
  4. temperatureto reflux for a further 2 hours
  5. washthe ether phase was washed with water, dilute sodium bicarbonate solution
  6. customAfter drying the organic phase
  7. customover sodium sulfate and evaporation under reduced pressure

出典と根拠

ORDレコード
ord-03e11201694046bcbabb459347e33315
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250517

反応ノート

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