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Ethyl Acetate → HCID 22375212、化合物

HRID 1956093
ノート
印刷プレビュー

反応式

HRID 1956093 の反応式
[CH2:1]([CH:6]1[CH2:11][CH2:10][CH:9]([CH:12]2[CH2:17][CH2:16][CH:15]([O:18][CH2:19][C:20](=[O:23])[CH2:21][CH3:22])[CH2:14][CH2:13]2)[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5].[H-].[H-].[H-].[H-].[Li+].[Al+3].C(OC(=O)C)C>C1COCC1>[CH2:1]([CH:6]1[CH2:11][CH2:10][CH:9]([CH:12]2[CH2:13][CH2:14][CH:15]([O:18][CH2:19][CH:20]([OH:23])[CH2:21][CH3:22])[CH2:16][CH2:17]2)[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5]
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 8857Ethyl AcetateHCID 21226445Aluminium lithium hydrideHCID 22375175HCID 22375175、化合物

生成物 1

HCID 22375212HCID 22375212、化合物収率 95%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

While keeping inside of a reaction system at a temperature of lower than 10° C., a solution of 5.24 g (16.3 mmol) of 4-(4-pentylcyclohexyl)-(2-oxobutyloxy)cyclohexane produced in Example 3 and dissolved in 35 ml of THF was added dropwise to a mixture of 0.46 g (12.2 mmol) of LAH and 2.5 ml of THF and further stirred for 5 hours at a room temperature. To this solution, under cooling, were added 5 ml of ethylacetate and then 10 ml of 2N aqueous solution of sodium hydroxide to terminate the reaction. After undissolved products were separated, the solvent was distilled off under a reduced pressure and the residue thus obtained was recrystallized from 15 ml of hexane to obtain 5.0 g (yield 95%) of 4-(4-pentylcyclohexyl)-(2-hydroxybutyloxy)cyclohexane.

後処理

  1. customlower than 10° C.
  2. temperatureTo this solution, under cooling
  3. custom10 ml of 2N aqueous solution of sodium hydroxide to terminate
  4. customthe reaction
  5. customAfter undissolved products were separated
  6. distillationthe solvent was distilled off under a reduced pressure
  7. customthe residue thus obtained
  8. customwas recrystallized from 15 ml of hexane

出典と根拠

ORDレコード
ord-39bb056ebece4225996da48174a41ebd
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05779936

反応ノート

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