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

HRID 1594862노트

반응식

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

참가 물질

반응물 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

생성물 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

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록: ord-c747706e699b4895b0ac98161f3d528b
출처 데이터셋: uspto-grants-2001_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06284755B1

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