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

HRID 1816763ノート

反応式

HRID 1816763 の反応式
[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

参加物

7

反応物 4

HCID 962WaterHCID 6328Methyl iodide2 回HCID 24758Sodium hydride2 回HCID 224947648-Cyclohexyl-1,4-dioxaspiro[4.5]decan-8-ol

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-b9d5e51fd8ea4585b578156732c5a7d9
出典データセット
uspto-grants-2005_04
特許番号
US06884868B1

反応ノート

読み込み中…