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

HRID 1811464Notes

Reaction equation

HRID 1811464 reaction equation
[ClH:1].[C:2]([C:5]1[S:6][CH:7]=[CH:8][CH:9]=1)(=[O:4])[CH3:3].Cl.[CH3:11][NH:12][CH3:13].[CH:14](O)(C)C>>[ClH:1].[CH3:11][N:12]([CH3:14])[CH2:13][CH2:3][C:2]([C:5]1[S:6][CH:7]=[CH:8][CH:9]=1)=[O:4]

Participants

5

Conditions

Temperature
77.5 °C

Procedure

Added 3.8 Kgs. of hydrochloric acid to a solution of 100 Kgs. of 2-acetyl thiophene, 81.5 Kgs. of dimethylamine hydrochloride, 35.4 Kgs. parafomaldehyde and 250 liters of isopropyl alcohol. Heated the reaction mixture to 75-80° C. Stirred the reaction mixture for 6 hours at 75-80° C. Cooled the reaction mixture to 0-5C. Stirred the reaction mixture for 2 hours at 0-5° C. Filtered the solid and washed with isopropyl alcohol.

Workup

  1. additionAdded 3.8 Kgs
  2. temperatureCooled the reaction mixture to 0-5C
  3. stirringStirred the reaction mixture for 2 hours at 0-5° C
  4. filtrationFiltered the solid
  5. washwashed with isopropyl alcohol

Sources & evidence

ORD record
ord-d58d7b419bbe403688afe0bc6b490db7
Source dataset
uspto-grants-2013_01
Patent number
US08362279B2

Reaction notes

Loading…