Water → HCID 19373306, 화합물

HRID 129323노트

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HRID 129323 반응식
[OH:1][CH2:2][C:3]1([CH2:11][OH:12])[CH2:8][O:7][C:6]([CH3:10])([CH3:9])[O:5][CH2:4]1.[H-].[Na+].[CH2:15](I)[CH3:16].O>CN(C)C=O>[CH3:10][C:6]1([CH3:9])[O:5][CH2:4][C:3]([CH2:11][O:12][CH2:15][CH3:16])([CH2:2][OH:1])[CH2:8][O:7]1

참가 물질

6

실험 절차

To a stirred solution of 5,5-di-(hydroxymethyl)-2,2-dimethyl-1,3dioxane (5.09) (Bellstein 19, II, 93) in dry dimethylformamide (50 ml) under nitrogen, at 20°, was added sodium hydride (0.689g, 80% dispersion in oil). The mixture was stirred at 80° for 2 hours and cooled. Ethyl iodide (4.49g) in dry dimethylformamide (40 ml) was added and the mixture was heated at 110° for 3 hours. The mixture was cooled and poured into water. The aqueous mixture was extracted with diethyl ether. The ethereal extracts were washed with brine, dried over anhydrous magnesium sulphate and evaporated in vacuo. 2,2-Dimethyl-5-ethoxymethyl-5- hydroxymethyl-1,3-dioxane was obtained as a pale yellow oil (1.2 g) and was used without further purification.

후처리

  1. temperaturecooled
  2. temperaturethe mixture was heated at 110° for 3 hours
  3. temperatureThe mixture was cooled
  4. extractionThe aqueous mixture was extracted with diethyl ether
  5. washThe ethereal extracts were washed with brine
  6. dry with materialdried over anhydrous magnesium sulphate
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-75883112f17b4ad99dff58ff1224eedc
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05466710

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