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Lithium Hydroxide → cis(+/-)-2-(4-{[(4-Chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-1H-benzimidazole-4-carboxylic acid

HRID 43809
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HRID 43809 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]3[NH:22][C:21]4[CH:23]=[CH:24][CH:25]=[C:26]([C:27]([O:29]C)=[O:28])[C:20]=4[N:19]=3)[CH2:14][C@H:13]2[O:31][CH3:32])=[O:10])[NH:5][C:6]=1[CH2:7][CH3:8].[OH-].[Li+]>CO.C1COCC1>[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]3[NH:22][C:21]4[CH:23]=[CH:24][CH:25]=[C:26]([C:27]([OH:29])=[O:28])[C:20]=4[N:19]=3)[CH2:14][C@H:13]2[O:31][CH3:32])=[O:10])[NH:5][C:6]=1[CH2:7][CH3:8]
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HCID 3939Lithium HydroxideHCID 86648755Methyl cis(+/-)-2-(4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-1H-benzimidazole-4-carboxylate

생성물 1

HCID 86648754cis(+/-)-2-(4-{[(4-Chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-1H-benzimidazole-4-carboxylic acid

시약·촉매·용매 2

HCID 887Methanol용매
HCID 8028
Tetrahydrofuran
용매

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온도
60 °C

실험 절차

Methyl cis(±)-2-(4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl)-1H-benzimidazole-4-carboxylate obtained in Example (187d) (190 mg, 0.41 mmol) was dissolved in methanol (5 ml) and THF (5 ml). A 2 N aqueous lithium hydroxide solution (5 ml) was added, and the mixture was stirred at 50 to 70° C. for one hour. The organic solvent was evaporated under reduced pressure, followed by neutralization with 1 N hydrochloric acid. The resulting solid was collected by filtration, washed with distilled water, and dried under reduced pressure at 45° C. to obtain the title compound as a solid.

후처리

  1. customThe organic solvent was evaporated under reduced pressure
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with distilled water
  4. customdried under reduced pressure at 45° C.

출처 및 근거

ORD 기록
ord-5234c57faf11428c8cdb2564f8f6e29f
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08536197B2

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