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

HRID 1462923

반응식

HRID 1462923 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.).

후처리

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

출처 및 근거

ORD 기록
ord-6dd396102f7743449c6ca1724ade3805
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04461902

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