(2-Ethyl-3-methoxybenzyl)dimethylamine → 3-Dimethylaminomethyl-2-ethylphenol hydrobromide

반응식

[CH2:1]([C:3]1[C:12]([O:13]C)=[CH:11][CH:10]=[CH:9][C:4]=1[CH2:5][N:6]([CH3:8])[CH3:7])[CH3:2].[BrH:15].C(O)(=O)C>>[BrH:15].[CH3:8][N:6]([CH2:5][C:4]1[C:3]([CH2:1][CH3:2])=[C:12]([OH:13])[CH:11]=[CH:10][CH:9]=1)[CH3:7]

참가 물질

반응물 2

HCID 13780987(2-Ethyl-3-methoxybenzyl)dimethylamine

HCID 21893785Acetic Acid Mixture with Hydrobromic Acid

생성물 1

HCID 137809943-Dimethylaminomethyl-2-ethylphenol hydrobromide수율 78%

실험 절차

(2-Ethyl-3-methoxybenzyl)dimethylamine (1.30 g, 6.73 mmol) was suspended in 30% hydrogen bromide/acetic acid (10 mL) and heated to reflux with stirring for 21 h. The cooled reaction mixture was triturated and decanted with successive portions of diethyl ether (3×), then triturated with diethyl ether overnight. The solid was collected by filtration, washed with ether and dried to give 3-dimethylaminomethyl-2-ethylphenol hydrobromide (1.37 g, 78%) as a tan solid.

후처리

temperatureheated
temperatureto reflux
customThe cooled reaction mixture
customwas triturated
customdecanted with successive portions of diethyl ether (3×)
customtriturated with diethyl ether overnight
filtrationThe solid was collected by filtration
washwashed with ether
customdried

출처 및 근거

ORD 기록: ord-77a9641dde704c4da36cca2d70d48e47
출처 데이터셋: uspto-grants-2007_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07276528B2

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