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Sodium Hydroxide → HCID 23295627、化合物

HRID 1953954
ノート
印刷プレビュー

反応式

HRID 1953954 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][CH:8]1[CH2:16][C:15]2[C:10](=[C:11]([CH3:20])[CH:12]=[CH:13][C:14]=2[CH:17]([CH3:19])[CH3:18])[C:9]1=[O:21].[OH-].[Na+]>C(OCC)C>[CH3:7][CH:8]1[CH2:16][C:15]2[C:10](=[C:11]([CH3:20])[CH:12]=[CH:13][C:14]=2[CH:17]([CH3:18])[CH3:19])[CH:9]1[OH:21]
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 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 22393249HCID 22393249、化合物

生成物 1

HCID 23295627HCID 23295627、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

In a 1-liter three-necked flask equipped with a 300-ml dropping funnel and a Dimroth condenser were charged 5.00 g (0.132 mol) of lithium aluminum hydride and 300 ml of diethyl ether, to which was dripped down at 0° C. over 1.5 hours about 50 g (0.25 mol) of 2,7-dimethyl-4-isopropyl-1-indanone diluted with 200 ml of diethyl ether. After stirring at room temperature for 30 minutes, the mixture was stirred under reflux for 1.5 hours. After completion of the reaction, 10 ml of ice water and 10 ml of aqueous sodium hydroxide solution were added at 0° C. and the resulting mixture was extracted with diethyl ether. The organic layer was washed with an aqueous sodium hydrogen carbonate solution and with saline and then dried over sodium sulfate. Sodium sulfate was removed by filtration and the solvent was distilled off under reduced pressure.

後処理

  1. customIn a 1-liter three-necked flask equipped with a 300-ml
  2. stirringthe mixture was stirred
  3. temperatureunder reflux for 1.5 hours
  4. additionwere added at 0° C.
  5. extractionthe resulting mixture was extracted with diethyl ether
  6. washThe organic layer was washed with an aqueous sodium hydrogen carbonate solution and with saline
  7. dry with materialdried over sodium sulfate
  8. customSodium sulfate was removed by filtration
  9. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-c776b5f855f342dca3eb6e5d1d802117
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06121182

反応ノート

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