Ethyl formate → 1-Formyl-4-(4-methoxyphenyl)piperazine

반응식

[OH2:1].Cl.Cl.C1(C[CH2:15][N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3OC)[CH2:18][CH2:17]2)C2C(=CC=CC=2)CCO1.[CH:30](OCC)=[O:31]>>[CH:15]([N:16]1[CH2:17][CH2:18][N:19]([C:22]2[CH:23]=[CH:24][C:25]([O:31][CH3:30])=[CH:26][CH:27]=2)[CH2:20][CH2:21]1)=[O:1]

참가 물질

반응물 2

HCID 8025Ethyl formate

HCID 232889511-[2-(Isochroman-1-yl)ethyl]-4-(2-methoxyphenyl)piperazine dihydrochloride monohydrate

생성물 1

HCID 232887711-Formyl-4-(4-methoxyphenyl)piperazine

실험 절차

A mixture of 1-(4-methoxyphenyl)piperazine (XI, 7.41 g) and ethyl formate (108 ml) is stirred at reflux for 3 hr. The mixture is then cooled, concentrated, and the residue chromatographed on silica gel eluting with methanol/dichloromethane (2/98). The appropriate fractions are pooled and concentrated to give 1-formyl-4-(4-methoxyphenyl)piperazine (VI), NMR (CDCl3) δ 3.05, 3.54, 3.71, 3.78, 6.88, 8.10.

후처리

temperatureat reflux for 3 hr
temperatureThe mixture is then cooled
concentrationconcentrated
customthe residue chromatographed on silica gel eluting with methanol/dichloromethane (2/98)
concentrationconcentrated

출처 및 근거

ORD 기록: ord-bf36939d21b241d38a0977748842d6d1
출처 데이터셋: uspto-grants-2000_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06133446

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