Dichloromethane → 4-[5-(2-Amino-ethyl)-2-methyl-imidazol-1-ylmethyl]-2-[3-(3-ethyl-1-methyl-2-oxo-azepan-3-yl)-phenoxy]-benzonitrile dihydrochloride

反応式

C(OC(=O)[NH:7][CH2:8][CH2:9][C:10]1[N:11]([CH2:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]#[N:24])=[C:19]([O:25][C:26]3[CH:31]=[CH:30][CH:29]=[C:28]([C:32]4([CH2:41][CH3:42])[CH2:38][CH2:37][CH2:36][CH2:35][N:34]([CH3:39])[C:33]4=[O:40])[CH:27]=3)[CH:18]=2)[C:12]([CH3:15])=[N:13][CH:14]=1)(C)(C)C.C(O)(C(F)(F)F)=O.C(Cl)[Cl:52]>>[ClH:52].[ClH:52].[NH2:7][CH2:8][CH2:9][C:10]1[N:11]([CH2:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]#[N:24])=[C:19]([O:25][C:26]3[CH:31]=[CH:30][CH:29]=[C:28]([C:32]4([CH2:41][CH3:42])[CH2:38][CH2:37][CH2:36][CH2:35][N:34]([CH3:39])[C:33]4=[O:40])[CH:27]=3)[CH:18]=2)[C:12]([CH3:15])=[N:13][CH:14]=1

参加物

反応物 3

HCID 6344Dichloromethane

HCID 6422Trifluoroacetic acid

HCID 54508564[2-(3-{4-cyano-3-[3-(3-ethyl-1-methyl-2-oxo-azepan-3-yl)-phenoxy]-benzyl}-2-methyl-3H-imidazol-4-yl)-ethyl]-carbamic acid tert-butyl ester

生成物 1

HCID 217062014-[5-(2-Amino-ethyl)-2-methyl-imidazol-1-ylmethyl]-2-[3-(3-ethyl-1-methyl-2-oxo-azepan-3-yl)-phenoxy]-benzonitrile dihydrochloride

実験手順

To a solution of [2-(3-{4-cyano-3-[3-(3-ethyl-1-methyl-2-oxo-azepan-3-yl)-phenoxy]-benzyl}-2-methyl-3H-imidazol-4-yl)-ethyl]-carbamic acid tert-butyl ester (as described in Step B above) (0.2 g, 0.41 mmol) in CH2Cl2 (6.0 mL) was added TFA (3.0 mL) and the solution was stirred for 0.5 hr. The solvents were removed in vacuo and the crude product was purified by preparative HPLC. Conversion to the HCl salt yielded the title compound.

後処理

customThe solvents were removed in vacuo
customthe crude product was purified by preparative HPLC

出典と根拠

ORDレコード: ord-c747706e699b4895b0ac98161f3d528b
出典データセット: uspto-grants-2001_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06284755B1

反応ノート

読み込み中…