Dichloromethane → 1-(4-tert-Butylphenyl)homopiperazine dihydrochloride, 98%

反応式

C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[CH:20]=[CH:19][C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O.[Cl:32]CCl>>[ClH:32].[C:21]([C:18]1[CH:17]=[CH:16][C:15]([N:11]2[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]2)=[CH:20][CH:19]=1)([CH3:24])([CH3:22])[CH3:23]

参加物

反応物 3

HCID 6344Dichloromethane

HCID 6422Trifluoroacetic acid

HCID 58576748HCID 58576748、化合物

生成物 1

HCID 666719201-(4-tert-Butylphenyl)homopiperazine dihydrochloride, 98%

実験手順

To 4-(4-tert-butyl-phenyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester (541 mg; 16.3 mmol, prepared in accordance with Example 160) is added a 2:3 mixture of trifluoroacetic acid and dichloromethane (5 mL) and the resulting reaction mixture is stirred at room temperature for 2 hours. All volatiles are then removed under high vacuum and the residue is taken up in a 4 molar solution of hydrochloric acid in dioxane. The solution is allowed to stand over night and the precipitate formed is filtered, washed (diethyl ether) and dried under high vacuum to afford the desired compound (452 mg) which is used in the next step without further purification.