Diethylamine → HCID 13318792, compound
Reaction equation
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[Cl:6][C@H:7]([CH3:11])[C:8](Cl)=[O:9]>C(Cl)(Cl)Cl>[CH2:1]([N:3]([CH2:4][CH3:5])[C:8](=[O:9])[C@H:7]([Cl:6])[CH3:11])[CH3:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Diethylamine (153 g) is added to a solution, maintained at 20° C., of (R)-2-chloropropionyl chloride (87.7 g) in chloroform (600 cc), in the course of 1 hour. The reaction mixture is washed with distilled water (500 cc), with an aqueous 1N hydrochloric acid solution (3×500 cc) and then with distilled water (500 cc). The organic phase is dried over sodium sulphate, filtered and then concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C. The residue obtained is distilled under reduced pressure (17 Pa). (R)-N,N-Diethyl-2-chloropropionamide (43 g) in the form of a colourless oil [b.p.17Pa =75°-80° C.; [α]D20 =-43.3° (c=10; CHCl3)] is thereby obtained.
Workup
- washThe reaction mixture is washed with distilled water (500 cc), with an aqueous 1N hydrochloric acid solution (3×500 cc)
- dry with materialThe organic phase is dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C
- customThe residue obtained
- distillationis distilled under reduced pressure (17 Pa)
Sources & evidence
- ORD record
- ord-32107fdb4918496db84cf57afef6f557
- Source dataset
- uspto-grants-1988_10
- Patent number
- US04775753
Reaction notes
Loading…