Sodium Carbonate → 1-(5,6,7,8-Tetrahydronaphthalen-1-yl)piperazine

HRID 481353

반응식

HRID 481353 반응식
[C:1]1([NH2:11])[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.Cl.Cl[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(O)CCC>[C:1]1([N:11]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 166715-TetralinylamineHCID 522769Bis(2-chloroethyl)amine hydrochloride

생성물 1

HCID 986981-(5,6,7,8-Tetrahydronaphthalen-1-yl)piperazine

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

5,6,7,8-Tetrahydronaphthalen-1-ylamine (1.4 ml, 15 mmol) is brought to the reflux point of 1-butanol (50 ml) in the presence of bis(2-chloroethyl)amine hydrochloride (2.68 g, 15 mmol) and sodium carbonate (800 mg, 7.5 mmol). After 48 h, the reaction mixture is concentrated and impregnated onto silica and then purified by flash chromatography with a mixture (95/5/1) and then (90/9/1) of dichloromethane/methanol/aqueous ammonia.

후처리

  1. concentrationthe reaction mixture is concentrated
  2. custompurified by flash chromatography with a mixture (95/5/1)

출처 및 근거

ORD 기록
ord-cf5b8c9e07c747c3ac0fadf998fe5196
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05789412

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