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

HRID 1282117노트

반응식

HRID 1282117 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 18423094Methyl 2-(4-aminomethylphenyl)-2-methylpropionate수율 68.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e1e5902d689740869b94c8493756d9eb
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455528B1

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