Water → 8-Cyclohexyl-8-methoxy-1,4-dioxaspiro[4.5]decane

HRID 1816763노트

반응식

HRID 1816763 반응식
[CH:1]1([C:7]2([OH:17])[CH2:16][CH2:15][C:10]3([O:14][CH2:13][CH2:12][O:11]3)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.I[CH3:19].[H-].[Na+].O>CN(C)C=O.ClCCl>[CH:1]1([C:7]2([O:17][CH3:19])[CH2:16][CH2:15][C:10]3([O:14][CH2:13][CH2:12][O:11]3)[CH2:9][CH2:8]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodide2회HCID 24758Sodium hydride2회HCID 224947648-Cyclohexyl-1,4-dioxaspiro[4.5]decan-8-ol

생성물 1

HCID 224947668-Cyclohexyl-8-methoxy-1,4-dioxaspiro[4.5]decane

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 8-cyclohexyl-1,4-dioxaspiro[4.5]decan-8-ol (1.143 g) and iodomethane (0.59 ml) in N,N-dimethylformamide (11 ml) was added sodium hydride (60% dispersion in mineral oil) (342 mg) at 0° C. The solution was stirred for 9 hours at 0° C., during which period additional iodomethane (0.59 ml) and sodium hydride (60% dispersion in mineral oil) (344 mg) was added to the mixture. The reaction mixture was added to a mixture of water and dichloromethane. The organic layer was washed with water. The organic layer was taken and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate elution) to give 8-cyclohexyl-8-methoxy-1,4-dioxaspiro[4.5]decane (1.201 g).

후처리

  1. additionwas added to the mixture
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationThe magnesium sulfate was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (ethyl acetate elution)

출처 및 근거

ORD 기록
ord-b9d5e51fd8ea4585b578156732c5a7d9
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06884868B1

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