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Sodium hydride → 2,2-Dimethyl-4-[(4-tetradecylphenoxy)methyl]-1,3-dioxolane

HRID 235716
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HRID 235716 반응식
[H-].[Na+].[CH2:3]([C:17]1[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=1)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].[CH3:24][C:25]1([CH3:36])[O:29][CH:28]([CH2:30]OS(C)(=O)=O)[CH2:27][O:26]1>CN(C)C=O.CCOCC>[CH3:24][C:25]1([CH3:36])[O:29][CH:28]([CH2:30][O:23][C:20]2[CH:19]=[CH:18][C:17]([CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])=[CH:22][CH:21]=2)[CH2:27][O:26]1
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참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 116800TetradecylphenolHCID 15570840(2,2-Dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate

생성물 1

HCID 202190872,2-Dimethyl-4-[(4-tetradecylphenoxy)methyl]-1,3-dioxolane

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide
용매

실험 절차

To a prewashed suspension of about 10.8 g of sodium hydride in about 800 ml of dimethylformamide was added about 43.5 g of 4-tetradecylphenol. The reaction was then refluxed about 2 hours, cooled to room temperature and about 37.8 g of freshly prepared 2,2-dimethyl-4-[[(methylsulfonyl)oxy]methyl]-1,3-dioxolane was added. The reaction was then refluxed for about 24 hours, cooled, diluted with ether, washed with water and dried, giving about 58.7 g of the desired title compound, mp 52°-53° C.

후처리

  1. temperatureThe reaction was then refluxed about 2 hours
  2. temperatureThe reaction was then refluxed for about 24 hours
  3. temperaturecooled
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-88815e8358ed408da13a89780dfa3a2a
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04640913

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