Trifluoroacetic acid methylene chloride → cis(+/-)-{(5Z)-5-[2-(4-{[(4-Chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-2-oxoethylidene]-2,4-dioxo-1,3-thiazolidin-3-yl}acetic acid

HRID 43758노트

반응식

HRID 43758 반응식
[Cl:1][C:2]1[N:3]=[C:4]([C:9]([NH:11][C@H:12]2[CH2:17][CH2:16][N:15]([C:18](=[O:35])/[CH:19]=[C:20]3/[C:21](=[O:34])[N:22]([CH2:26][C:27]([O:29]C(C)(C)C)=[O:28])[C:23](=[O:25])[S:24]/3)[CH2:14][C@H:13]2[O:36][CH3:37])=[O:10])[NH:5][C:6]=1[CH2:7][CH3:8].FC(F)(F)C(O)=O.ClCCl>CO>[Cl:1][C:2]1[N:3]=[C:4]([C:9]([NH:11][C@H:12]2[CH2:17][CH2:16][N:15]([C:18](=[O:35])/[CH:19]=[C:20]3/[C:21](=[O:34])[N:22]([CH2:26][C:27]([OH:29])=[O:28])[C:23](=[O:25])[S:24]/3)[CH2:14][C@H:13]2[O:36][CH3:37])=[O:10])[NH:5][C:6]=1[CH2:7][CH3:8]

참가 물질

4

반응물 2

HCID 21863450Trifluoroacetic acid methylene chlorideHCID 86648706tert-Butyl cis(+/-)-{(5Z)-5-[2-(4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-2-oxoethylidene]-2,4-dioxo-1,3-thiazolidin-3-yl}acetate

생성물 1

HCID 86648705cis(+/-)-{(5Z)-5-[2-(4-{[(4-Chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-2-oxoethylidene]-2,4-dioxo-1,3-thiazolidin-3-yl}acetic acid수율 43%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

tert-Butyl cis(±)-{(5Z)-5-[2-(4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-2-oxoethylidene]-2,4-dioxo-1,3-thiazolidin-3-yl}acetate obtained in Example (163a) (20.4 mg, 0.04 mmol) was dissolved in methanol (4 mL). A 20% trifluoroacetic acid-dichloromethane solution (5 ml) was added, and the mixture was stirred at room temperature. The organic solvent was evaporated under reduced pressure, and then the residue was washed with ether. The solid was collected by filtration to obtain 7.79 mg of the title compound as a white solid (43%).

후처리

  1. customThe organic solvent was evaporated under reduced pressure
  2. washthe residue was washed with ether
  3. filtrationThe solid was collected by filtration

출처 및 근거

ORD 기록
ord-8a46873355bd4fe596100f9b93b7f1d5
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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