Hydrochloric Acid → HCID 67437276, compound
Reaction equation
[ClH:1].C1(C(=[N:15][N:16]2[CH:20]([CH3:21])[CH2:19][CH2:18][C:17]2=[O:22])C2C=CC=CC=2)C=CC=CC=1.C(OCC)(=O)C>O1CCCC1>[Cl-:1].[CH3:21][CH:20]1[CH2:19][CH2:18][C:17](=[O:22])[N:16]1[NH3+:15]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
At room temperature 50 ml of 37% strength hydrochloric acid are added to a solution of 17.8 g (63.9 mmol) of 1-[(diphenylmethylene)amino]-5-methylpyrrolidin-2-one in 100 ml of tetrahydrofuran, and the mixture is stirred for 1 h. Ethyl acetate is then added to the reaction mixture, and the organic phase is separated off. Repeatedly, ethanol/toluene (1:1) is added to the hydrochloric acid phase and the mixture is concentrated under reduced pressure. The crude product obtained is reacted further without further purification. 1H-NMR (ppm): δ (DMSO-d6)=1.24 (d, 3H), 1.60-1.65 (m, 1H), 2.20-2.42 (m, 3H), 3.88 (m, 1H).
Workup
- customthe organic phase is separated off
- additionRepeatedly, ethanol/toluene (1:1) is added to the hydrochloric acid phase
- concentrationthe mixture is concentrated under reduced pressure
Sources & evidence
- ORD record
- ord-2f3826acb758469ea73894f14ad0c17a
- Source dataset
- uspto-grants-2013_08
- Patent number
- US08507472B2
Reaction notes
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