Sodium Hydroxide → N-ethyl-1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine hydrochloride
반응식
[BH4-].[Na+].[Cl:3][C:4]1C=C(C2(C(N)C)CCC2)C=C[C:9]=1Cl.Cl.[Cl:19][C:20]1[CH:21]=[C:22]([C:27]2([CH:31]([NH2:33])[CH3:32])[CH2:30][CH2:29][CH2:28]2)[CH:23]=[CH:24][C:25]=1[Cl:26].[OH-].[Na+]>C(O)(=O)C>[ClH:3].[CH2:4]([NH:33][CH:31]([C:27]1([C:22]2[CH:23]=[CH:24][C:25]([Cl:26])=[C:20]([Cl:19])[CH:21]=2)[CH2:30][CH2:29][CH2:28]1)[CH3:32])[CH3:9]참가 물질
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
Sodium borohydride (2.0 g) was added to solution of 1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine (1.5 g prepared by treating the product of Example 1 with aqueous sodium hydroxide) in glacial acetic acid (30 ml). The mixture was heated at 95°-100° C. for sixteen hours and then cooled. Aqueous sodium hydroxide solution was added and the reaction mixture extracted with ether. The ether extract was shaken with 5N hydrochloric acid and the aqueous layer was washed with ether, basified and extracted with ether. Hydrogen chloride gas was passed into the ether extract which was evaporated to dryness. Trituration with acetone gave N-ethyl-1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine hydrochloride (m.p. 211°-212° C.). (Formula I R1 =Me; R2 =H; R3 =Et; R4 =H; R5 =4-Cl and R6 =3-Cl.)
후처리
- customprepared
- temperatureThe mixture was heated at 95°-100° C. for sixteen hours
- temperaturecooled
- extractionthe reaction mixture extracted with ether
- extractionThe ether extract
- washthe aqueous layer was washed with ether
- extractionextracted with ether
- extractionextract which
- customwas evaporated to dryness
출처 및 근거
- ORD 기록
- ord-7a786213d40b494193464548902d91d9
- 출처 데이터셋
- uspto-grants-1985_06
- 특허 번호
- US04522828
반응 노트
불러오는 중…