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

HRID 1194441Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1194441
[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]ethylamine. 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-(3,4dichlorophenyl)cyclobutyl]ethylamine hydrochloride (m.p. 185°-195° C.). (Formula I R1 =Me; 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-c3c0a3ddbe1945bb9e3b3a45beb6fd6b
Quelldatensatz
uspto-grants-1989_03
Patentnummer
US04814352

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