Water → HCID 19373306, 화합물

HRID 1197376노트

반응식

HRID 1197376 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

반응물 4

HCID 962WaterHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 373708NSC650609

생성물 1

HCID 19373306HCID 19373306, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a stirred solution of 5,5-di-(hydroxymethyl)-2,2-dimethyl-1,3-dioxane (5.0 g) (Beilstein 19, II, 93) in dry dimethylformamide (50 ml) under nitrogen, at 20°, was added sodium hydride (0.68 g, 80% dispersion in oil). The mixture was stirred at 80° for 2 hours and cooled. Ethyl iodide (4.4 g) 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-b5a1b2e458c44ca5ac34c337b2034a59
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05116862

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