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

HRID 218256ノート

反応式

HRID 218256 の反応式
[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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 15413tert-Butyl methyl ether溶媒HCID 21901440N,N-dimethylformamide methanol溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-6784459a6cf742198cf58dd9d711a4f5
出典データセット
uspto-grants-2012_06
特許番号
US08198302B2

反応ノート

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