Tetrahydrofuran → Methyl 2-(4-aminomethylphenyl)-2-methylpropionate

HRID 1282117ノート

反応式

HRID 1282117 の反応式
[N:1]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]([CH3:17])([CH3:16])[C:12]([O:14][CH3:15])=[O:13])=[CH:7][CH:6]=1)=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O1CCCC1>O>[NH2:1][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]([CH3:17])([CH3:16])[C:12]([O:14][CH3:15])=[O:13])=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 11776TriphenylphosphineHCID 18423002Methyl 2-(4-azidomethylphenyl)-2-methylpropionate

生成物 1

HCID 18423094Methyl 2-(4-aminomethylphenyl)-2-methylpropionate収率 68.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of methyl 2-(4-azidomethylphenyl)-2-methylpropionate (48.1 g)and triphenylphosphine (59.5 g) in a mixed solvent of tetrahydrofuran (480 ml) and water (24 ml) was refluxed for 30 min. The solvent was evaporated, and the obtained residue was purified by silica gel column chromatography (developing solvent; chloroform:methanol=10:1, chloroform:methanol:aqueous ammonia=10:1:0.3) to give the title compound (29.4 g) as a pale-yellow oil.

後処理

  1. customThe solvent was evaporated
  2. customthe obtained residue was purified by silica gel column chromatography (developing solvent; chloroform:methanol=10:1, chloroform:methanol:aqueous ammonia=10:1:0.3)

出典と根拠

ORDレコード
ord-e1e5902d689740869b94c8493756d9eb
出典データセット
uspto-grants-2002_09
特許番号
US06455528B1

反応ノート

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