Potassium Fluoride → 4-Phenyl-6-[(z)-2-(3,4,5-trimethoxyphenyl)vinyl]-1,2-dihydroxybenzene

HRID 218256노트

반응식

HRID 218256 반응식
[C:1]1([C:7]2[CH:12]=[C:11](/[CH:13]=[CH:14]\[C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[C:17]([O:25][CH3:26])[CH:16]=3)[C:10]([O:27][Si](C(C)(C)C)(C)C)=[C:9]([O:35][Si](C(C)(C)C)(C)C)[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[F-].[K+]>CO.CN(C)C=O.C(O)(=O)C.C(OC)(C)(C)C>[C:1]1([C:7]2[CH:12]=[C:11](/[CH:13]=[CH:14]\[C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[C:17]([O:25][CH3:26])[CH:16]=3)[C:10]([OH:27])=[C:9]([OH:35])[CH:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 2

HCID 522689Potassium FluorideHCID 601306744-Phenyl-6-[(Z)-2-(3,4,5-trimethoxyphenyl)vinyl]-1,2-di(tert-butyldimethylsilyloxy)benzene

생성물 1

HCID 99997064-Phenyl-6-[(z)-2-(3,4,5-trimethoxyphenyl)vinyl]-1,2-dihydroxybenzene

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 15413tert-Butyl methyl ether용매HCID 21901440N,N-dimethylformamide methanol용매

실험 절차

To a solution of 24 (0.05 g, 0.082 mmol) in methanol:dimethylformamide 1:1 (2 mL), acetic acid was added (0.025 mL, 0.41 mmol) followed by potassium fluoride (0.024 mg, 0.41 mmol). The mixture was stirred for 6 hours then diluted with tertbutylmethyl ether (50 mL) and washed with water (10 mL) then brine (50 mL), then dried over sodium sulphate. The solvent was removed under reduced pressure to give a crude which was purified by column (cyclohexane:AcOEt 6:4+1% AcOH) to give 0.097 g of ZSB-80:

후처리

  1. washwashed with water (10 mL)
  2. dry with materialbrine (50 mL), then dried over sodium sulphate
  3. customThe solvent was removed under reduced pressure
  4. customto give a crude which
  5. customwas purified by column (cyclohexane:AcOEt 6:4+1% AcOH)
  6. customto give 0.097 g of ZSB-80

출처 및 근거

ORD 기록
ord-6784459a6cf742198cf58dd9d711a4f5
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198302B2

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