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

HRID 481353

反応式

HRID 481353 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-cf5b8c9e07c747c3ac0fadf998fe5196
出典データセット
uspto-grants-1998_08
特許番号
US05789412

関連ノート

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