Acetone → 3,5-Di(3,5-di(4-vinylbenzyloxy)benzyloxy)benzylalcohol

HRID 322606

반응식

HRID 322606 반응식
[CH:1]([C:3]1[CH:28]=[CH:27][C:6]([CH2:7][O:8][C:9]2[CH:10]=[C:11]([CH:14]=[C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][C:22]([CH:25]=[CH2:26])=[CH:21][CH:20]=3)[CH:16]=2)[CH2:12]Br)=[CH:5][CH:4]=1)=[CH2:2].[CH3:29][C:30]([CH3:32])=[O:31].[OH:33][C:34]1[CH:35]=[C:36]([CH:39]=[C:40]([OH:42])[CH:41]=1)[CH2:37][OH:38].[C:43]([O-:46])([O-])=O.[K+].[K+]>C1(C)C=CC=CC=1.CCCCCC.O.C(Cl)Cl>[CH:1]([C:3]1[CH:28]=[CH:27][C:6]([CH2:7][O:8][C:9]2[CH:10]=[C:11]([CH:14]=[C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][C:22]([CH:25]=[CH2:26])=[CH:21][CH:20]=3)[CH:16]=2)[CH2:12][O:31][C:30]2[CH:32]=[C:16]([CH:9]=[C:10]([O:38][CH2:37][C:36]3[CH:35]=[C:34]([O:33][CH2:18][C:19]4[CH:24]=[CH:23][C:22]([CH:25]=[CH2:26])=[CH:21][CH:20]=4)[CH:41]=[C:40]([O:42][CH2:7][C:6]4[CH:5]=[CH:4][C:3]([CH:1]=[CH2:2])=[CH:28][CH:27]=4)[CH:39]=3)[CH:29]=2)[CH2:43][OH:46])=[CH:5][CH:4]=1)=[CH2:2]

참가 물질

9

반응물 4

HCID 180AcetoneHCID 11430Potassium CarbonateHCID 346613,5-Dihydroxybenzyl alcoholHCID 184339453,5-Bis(4-vinylbenzyloxy)benzyl bromide

생성물 1

HCID 184339443,5-Di(3,5-di(4-vinylbenzyloxy)benzyloxy)benzylalcohol수율 81.9%

시약·촉매·용매 4

HCID 962Water용매HCID 1140Toluene용매HCID 6344Dichloromethane용매HCID 8058Hexane용매

실험 절차

A 250 ml flask is charged with 15 g (34.5 mmol, 2.2 eq) of bromide (2) and acetone (100 ml) under an argon atmosphere. To this solution is added 3,5-dihydroxybenzyl alcohol (2.2 g, 15.7 mmol), 0.82 g (31. mmol, 0.2 eq) 18-C-6 and 4.77 g (34-5 mmol, 2.2 eq) of K2CO3 and the mixture is stirred for 48 hours whereupon a yellow suspension is formed. To the mixture is added methylene chloride (200 ml) and water (200 ml). The organic phase is separated, dried over MgSO4 and evaporated to dryness. A dark brown oil is obtained which is dissolved in toluene (40 ml) and hexane (20 ml). Upon cooling, a white powder forms which is collected by filtration to give 10.92 g (81.9% of (3A).

후처리

  1. customis formed
  2. customThe organic phase is separated
  3. dry with materialdried over MgSO4
  4. customevaporated to dryness
  5. customA dark brown oil is obtained which
  6. temperatureUpon cooling
  7. filtrationa white powder forms which is collected by filtration

출처 및 근거

ORD 기록
ord-7c38a8d86c804a088e9b4407bbaf07ed
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211316B1

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