Water → (8-Methyl-1,4-dioxaspiro(4.5)decan-8-yl)methanol

HRID 1462923

反応式

HRID 1462923 の反応式
[CH2:1]1[CH2:15][O:14][C:3]2([CH2:8][CH2:7][C:6]([CH3:13])([C:9](OC)=[O:10])[CH2:5][CH2:4]2)[O:2]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].C(OCC)(=O)C.O>CCOCC>[CH2:15]1[CH2:1][O:2][C:3]2([CH2:4][CH2:5][C:6]([CH3:13])([CH2:9][OH:10])[CH2:7][CH2:8]2)[O:14]1

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 21226445Aluminium lithium hydrideHCID 22591390Methyl 8-methyl-1,4-dioxaspiro[4.5]decane-8-carboxylate

生成物 1

HCID 12568263(8-Methyl-1,4-dioxaspiro(4.5)decan-8-yl)methanol収率 89.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

The thus-obtained methyl 4,4-ethylenedioxy-1-methylcyclohexanecarboxylate (37.8 g) was dissolved in ether (100 ml), and the solution was added dropwise to a refluxing suspension of LiAlH4 (6.7 g) in ether (400 ml). After the addition, the mixture was stirred at room temperature for an hour and then cooled with ice. Ethyl acetate (20 ml) and then water (35 ml) were added dropwise cautiously thereto. The solid precipitate was filtered off, and the filtrate was distilled under reduced pressure to give 4,4-ethylenedioxy-1-methylcyclohexanemethanol (29.5 g, 89.9% yield, b.p. 120°-125° C./0.5 mmHg, m.p. 42°-43° C.).

後処理

  1. additionAfter the addition
  2. temperaturecooled with ice
  3. filtrationThe solid precipitate was filtered off
  4. distillationthe filtrate was distilled under reduced pressure

出典と根拠

ORDレコード
ord-6dd396102f7743449c6ca1724ade3805
出典データセット
uspto-grants-1984_07
特許番号
US04461902

関連ノート

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