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Water → 8-Methoxy-8-(methoxymethyl)-1,4-dioxaspiro[4.5]decane

HRID 922119
ノート
印刷プレビュー

反応式

HRID 922119 の反応式
[CH3:1][O:2][CH2:3][C:4]1([OH:14])[CH2:13][CH2:12][C:7]2([O:11][CH2:10][CH2:9][O:8]2)[CH2:6][CH2:5]1.[H-].[Na+].I[CH3:18].O>O1CCCC1>[CH3:18][O:14][C:4]1([CH2:3][O:2][CH3:1])[CH2:13][CH2:12][C:7]2([O:8][CH2:9][CH2:10][O:11]2)[CH2:6][CH2:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodide2 回HCID 24758Sodium hydrideHCID 712472648-(Methoxymethyl)-1,4-dioxaspiro[4.5]decan-8-ol

生成物 1

HCID 712474008-Methoxy-8-(methoxymethyl)-1,4-dioxaspiro[4.5]decane

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3.40 g (16.8 mmol) of the compound from Example 8A were dissolved in 170 ml of tetrahydrofuran, 1.01 g (25.2 mmol) of sodium hydride (60% in paraffin oil) were added and the mixture was stirred at room temperature for 0.5 hour. 3.58 g (25.2 mmol) of iodomethane were then added, and the reaction mixture was stirred at room temperature for two hours. 3.58 g (25.2 mmol) of iodomethane were then added, and the reaction mixture was stirred at room temperature for two hours. Water was added, the mixture was extracted repeatedly with ethyl acetate and the combined organic phases were dried over sodium sulphate, filtered and concentrated. This gave 3.35 g (92% of theory) of the title compound.

後処理

  1. stirringthe reaction mixture was stirred at room temperature for two hours
  2. stirringthe reaction mixture was stirred at room temperature for two hours
  3. extractionthe mixture was extracted repeatedly with ethyl acetate
  4. dry with materialthe combined organic phases were dried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-32958f47d1264cd592b62c6285ed0d1f
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278925B2

反応ノート

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