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

HRID 1194441ノート

反応式

HRID 1194441 の反応式
[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]

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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).

後処理

  1. customconcentrated hydrochloric acid and the solution evaporated to dryness

出典と根拠

ORDレコード
ord-c3c0a3ddbe1945bb9e3b3a45beb6fd6b
出典データセット
uspto-grants-1989_03
特許番号
US04814352

反応ノート

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