Formaldehyde → 1-(1-Ethyl-1H-pyrrol-2-yl)-N,N-dimethylmethanamine

A mixture of a 35% aqueous formaldehyde solution (9.0 mL, 105 mmol) and dimethylamine hydrochloride (9.0 g, 110 mmol) was added to 1-ethylpyrrol (10.0 g, 105 mmol) under ice-cooling with stirring over 1 hour and 30 minutes and the mixture was stirred at room temperature for 6 hours. A 10% aqueous sodium hydroxide solution (150 mL) and ether were added to the reaction mixture to separate it. The thus obtained organic phase was separated, washed with a saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure and the residue was purified by silica gel chromatography (methylene chloride:methanol, 9:1) to obtain 2-(N,N-dimethylaminomethyl)-1-ethylpyrrol (15.6 9, yield: 97%).

1. temperaturecooling
2. stirringthe mixture was stirred at room temperature for 6 hours
3. customto separate it
4. customThe thus obtained organic phase was separated
5. washwashed with a saturated aqueous NaCl solution
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationAfter filtration
8. customthe solvent was evaporated under reduced pressure
9. customthe residue was purified by silica gel chromatography (methylene chloride:methanol, 9:1)

ORDレコード

ord-eb81db39084e4ab794d972745fa2042f

出典データセット

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07910617B2