5-Bromo-1,2,3-trimethoxybenzene → HCID 178418846、化合物

HRID 9310

反応式

HRID 9310 の反応式
C([Li:5])CCC.[CH3:6][O:7][C:8]1[CH:9]=[C:10](Br)[CH:11]=[C:12]([O:16][CH3:17])[C:13]=1[O:14][CH3:15]>CCOCC>[CH3:6][O:7][C:8]1[CH:9]=[C:10]([Li:5])[CH:11]=[C:12]([O:16][CH3:17])[C:13]=1[O:14][CH3:15]

参加物

4

反応物 2

HCID 758855-Bromo-1,2,3-trimethoxybenzeneHCID 178418339Butyllithium

生成物 1

HCID 178418846HCID 178418846、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a stirred solution of n-butyllithium (3.7 mL, 1.6 M in hexane solution,6.0 mol) in dry ether (40 mL), a solution of 3,4,5-trimethoxyphenylbromide (0.74 g, 3.0 mol) in ether (20 mL) was added under dry nitrogen at −78° C. The solution was stirred for 1 h in order to form 3,4,5-trimethoxyphenyllithum (“TPL”). Substituted tetralone reagent (3.0 mol) was added at −20° C., and the stirring was continued for 2 h (−20° C.-RT). The mixture was partitioned between CH2Cl2 and water, the organic layer was dried over anhydrous sodium sulfate, and, after filtration, the organic layer was concentrated in vacuo to provide a tetrahydronaphthalen-1-ol as a yellow oil. Each compound was purified by column chromatography.

出典と根拠

ORDレコード
ord-44b54a3e212a410d8860722b1d5535c3
出典データセット
uspto-grants-2006_08
特許番号
US07091240B2

関連ノート

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