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

HRID 35696노트

반응식

HRID 35696 반응식
[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]

참가 물질

3

반응물 1

HCID 130831401-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine

생성물 1

HCID 130831411-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine hydrochloride

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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-(3,4-dichlorophenyl)cyclobutyl]ethylamine hydrochloride (m.p. 185°-195° C.). (Formula I R1 =Me; R2,R3 and R4 =H; R5 =4--Cl; R6 =3--Cl).

후처리

  1. customconcentrated hydrochloric acid and the solution evaporated to dryness

출처 및 근거

ORD 기록
ord-30dd2d099b8045a4b4c0ff309688b6c1
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767790

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