Hydrogen chloride-ethyl acetate → 1-(2,4-Dimethylphenyl)-[1,4]diazepane hydrochloride

HRID 1804035노트

반응식

HRID 1804035 반응식
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:16]=2[CH3:22])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:23].C(OCC)(=O)C>C(Cl)(Cl)Cl>[ClH:23].[CH3:22][C:16]1[CH:17]=[C:18]([CH3:21])[CH:19]=[CH:20][C:15]=1[N:11]1[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]1

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 673808924-(2,4-Dimethylphenyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester

생성물 1

HCID 673808831-(2,4-Dimethylphenyl)-[1,4]diazepane hydrochloride

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To 1-bromo-2,4-dimethylbenzene (1.85 g) were added 1-BOC-1,4]diazepane (2 g), palladium (II) acetate (0.115 g), rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (0.31 g), sodium tert-butoxide (1.34 g) and toluene (35 mL), and the mixture was refluxed for 9 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The residue was purified by column chromatography (chloroform:methanol) to give 4-(2,4-dimethylphenyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester (2.16 g). To 4-(2,4-dimethylphenyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester (2.16 g) were added 4N hydrogen chloride/ethyl acetate (6.9 mL) and chloroform (17 mL), and the mixture was stirred at room temperature overnight. The solvent was evaporated to give the title compound (1.74 g).

후처리

  1. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-845ccd21ee304c4cadc6402690ab41fa
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354401B2

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