Hydrochloric Acid → 3-(Dimethylamino)-1-(thiophen-2-yl)propan-1-one hydrochloride

温度

70 °C

To a stirred solution of 37% HCl (0.60 mL, 19.8 mmol, 0.5 equivalents) in 2-propanol (73 mL) were added paraformaldehyde (3.00 gm, 95.1 mmol, 2.4 equivalents), dimethylamine hydrochloride (8.07 gm, 99.0 mmol, 2.5 equivalents) and 2-acetylthiophene (5.0 gm, 39.6 mmol) in sequence at room temperature. The cloudy suspension was heated to 70° C., gradually turning to a clear homogenous mixture. After approximately 18 h at 70° C. a white precipitate had formed. The reaction mixture was cooled to room temperature, and the white solid was filtered and washed with ice-cold ethanol (2×30 mL). The white solid was dried in a vacuum oven at 50° C. for 12 h to give 6.0 gm (69%) of 1 as a white solid.

1. customAfter approximately 18 h at 70° C. a white precipitate had formed
2. temperatureThe reaction mixture was cooled to room temperature
3. filtrationthe white solid was filtered
4. washwashed with ice-cold ethanol (2×30 mL)
5. customThe white solid was dried in a vacuum oven at 50° C. for 12 h

ORDレコード

ord-147752c11c96417ba777a98d6cf7acf9

出典データセット

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09233165B2