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

HRID 922119
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HRID 922119 반응식
[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
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참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodide2회HCID 24758Sodium hydrideHCID 712472648-(Methoxymethyl)-1,4-dioxaspiro[4.5]decan-8-ol

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-32958f47d1264cd592b62c6285ed0d1f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278925B2

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