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Triphenylphosphine → 2-Hydroxy-4-(2-methoxy-4-vinylphenyl)-4-methyl-2-trifluoromethylvaleric acid methyl ester

HRID 1869387
ノート
印刷プレビュー

反応式

HRID 1869387 の反応式
[CH3:1][O:2][C:3](=[O:23])[C:4]([OH:22])([C:18]([F:21])([F:20])[F:19])[CH2:5][C:6]([C:9]1[CH:14]=[CH:13][C:12](I)=[CH:11][C:10]=1[O:16][CH3:17])([CH3:8])[CH3:7].[CH2:24](C([Sn])=C(CCCC)CCCC)[CH2:25]CC.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[CH3:1][O:2][C:3](=[O:23])[C:4]([OH:22])([C:18]([F:21])([F:20])[F:19])[CH2:5][C:6]([C:9]1[CH:14]=[CH:13][C:12]([CH:24]=[CH2:25])=[CH:11][C:10]=1[O:16][CH3:17])([CH3:8])[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11776TriphenylphosphineHCID 179892492-Hydroxy-4-(4-iodo-2-methoxyphenyl)-4-methyl-2-trifluoromethyl-valeric acid methyl esterHCID 53438229Tri(butyl)vinyltin

生成物 1

HCID 179893052-Hydroxy-4-(2-methoxy-4-vinylphenyl)-4-methyl-2-trifluoromethylvaleric acid methyl ester収率 43.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

1 g of 2-hydroxy-4-(4-iodo-2-methoxyphenyl)-4-methyl-2-trifluoromethyl-valeric acid methyl ester, 860 mg of tributylvinyl tin, 103 mg of palladium-dibenzylidene acetone complex and 30 mg of triphenylphosphine in 17 ml of THF are refluxed under argon atmosphere for 57 hours. It is filtered through diatomaceous earth and completely concentrated by evaporation. After chromatography on silica gel (hexane/ethyl acetate 0->2%), 339 mg of 2-hydroxy-4-(2-methoxy-4-vinylphenyl)-4-methyl-2-trifluoromethylvaleric acid methyl ester is obtained. The latter is stirred with 56 mg of lithium aluminum hydride in 11 ml of diethyl ether at room temperature for 10 hours. It is added to saturated bicarbonate solution, filtered through diatomaceous earth and extracted with ethyl acetate. The organic phase is washed with bicarbonate solution and brine, dried (Na2SO4) and concentrated by evaporation. After chromatography on silica gel (hexane/ethyl acetate 0->10%), 148 mg of 2-hydroxy-4-(2-methoxy-4-vinylphenyl)-4-methyl-2-trifluoro-methylpentanol is obtained. The latter is hydrogenated in 4.3 ml of ethyl acetate with 14 mg of palladium on activated carbon under normal pressure with hydrogen. The batch is filtered through diatomaceous earth and completely concentrated by evaporation. 127 mg of 4-(4-ethyl-2-methoxyphenyl)-2-hydroxy-4-methyl-2-trifluoromethylpentanol is obtained. The diol that is obtained is reacted with 0.29 ml of triethylamine and 280 mg of sulfur trioxide-pyridine complex in 1.3 ml of DMSO at room temperature in 10 hours of reaction time. It is added to saturated ammonium chloride solution and extracted with ethyl acetate. The organic phase is washed with water and brine, dried (Na2SO4) and concentrated by evaporation in a vacuum. After chromatography on silica gel (hexane/ethyl acetate 0->3%), 94 mg of the title compound is obtained as a colorless oil.

後処理

  1. filtrationIt is filtered through diatomaceous earth
  2. concentrationcompletely concentrated by evaporation

出典と根拠

ORDレコード
ord-2914f742bb794c6bb0cf891b6832ec2f
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07638515B2

反応ノート

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