1-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine → 1-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine hydrochloride

HRID 1248127Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1248127
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH:13]([NH2:15])[CH3:14])[CH2:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]>CC(O)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH:13]([NH2:15])[CH3:14])[CH2:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

Komponenten

3

Versuchsvorschrift

1-Acetyl-1-(3,4-dichlorophenyl)cyclobutane (9.1 g) prepared as above, formamide (6.5 ml) and 98% formic acid (3 ml) were heated at 180° C. for sixteen hours to give N-formyl-1-[1-(3,4-dichlorophenyl)cyclobutyl]ethlyamine. Concentrated hydrochloric acid (20 ml) was added and the mixture heated under reflux for three hours. The solution was then cooled, washed with ether and sodium hydroxide solution added. The product was extracted with ether, and the ether extract washed with water, dried and evaporated. 1-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine (b.p. 112°-118° at 0.2 mm Hg) was isolated by distillation. The amine was dissolved in propan-2-ol and concentrated hydrochloric acid and the solution evaporated to dryness to give 1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine hydrochloride (m.p. 185°-195° C.). (Formula I R1 =M3; R2,R3 and R4 =H; R5 =4-Cl; R6 =3-Cl).

Aufarbeitung

  1. customconcentrated hydrochloric acid and the solution evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-3aa6f80f633a446b89cfba5f33ebcc88
Quelldatensatz
uspto-grants-1985_06
Patentnummer
US04522828

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