Hydrochloric Acid → HCID 178496730, 화합물

HRID 1099471노트

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HRID 1099471 반응식
C([O:3][C:4](=[O:41])[CH2:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([NH:12][C:13](=[O:40])[CH:14]([CH:34]2[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]2)[N:15]2[C:19]3[CH:20]=[CH:21][C:22]([F:24])=[CH:23][C:18]=3[N:17]=[C:16]2[C@H:25]([O:32][CH3:33])[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH2:8][CH2:7]1)C.[Li+].[OH-].Cl>C(#N)C>[CH:34]1([CH:14]([N:15]2[C:19]3[CH:20]=[CH:21][C:22]([F:24])=[CH:23][C:18]=3[N:17]=[C:16]2[C@H:25]([O:32][CH3:33])[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:13]([NH:12][C@H:9]2[CH2:8][CH2:7][C@H:6]([CH2:5][C:4]([OH:41])=[O:3])[CH2:11][CH2:10]2)=[O:40])[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 178471810HCID 178471810, 화합물

생성물 1

HCID 178496730HCID 178496730, 화합물수율 76%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
110 °C

실험 절차

To a solution of (trans-4-{2-cyclohexyl-2-[5-fluoro-2-((R)-methoxy-phenyl-methyl)-benzoimidazol-1-yl]-acetylamino}-cyclohexyl)-acetic acid ethyl ester (190 mg, 0.34 mmol, 1.0 equiv) in acetonitrile (3 mL) was added a solution of 1 M LiOH (2 mL) and the reaction mixture heated by microwave irradiation to 110° C. for 30 min. A solution of 1 M HCl (25 mL) was added, the organic solvents removed by evaporation under reduced pressure and the residue extracted with ethyl acetate. The organic layer was washed with water, dried over Na2SO4 and concentrated by evaporation under reduced pressure yielding 138 mg (76%) of the title compound. MS (ISP): 536.4 [M+H]+.

후처리

  1. customthe organic solvents removed by evaporation under reduced pressure
  2. extractionthe residue extracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-42495dc82c9e4c638eedddaddafd1b34
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143422B2

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