Lithium Hydroxide → 2-(4-((tert-butoxycarbonyl)amino)-1H-indazol-1-yl)-2-(4-chlorophenyl)butanoic acid

HRID 1477895노트

반응식

HRID 1477895 반응식
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH:11]=[N:12][N:13]2[C:18]([C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=1)([CH2:23][CH3:24])[C:19]([O:21]C)=[O:20])=[O:7])([CH3:4])([CH3:3])[CH3:2].[Li+].[OH-]>O1CCOCC1.O>[C:1]([O:5][C:6]([NH:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH:11]=[N:12][N:13]2[C:18]([C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=1)([CH2:23][CH3:24])[C:19]([OH:21])=[O:20])=[O:7])([CH3:2])([CH3:3])[CH3:4]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 70562967methyl 2-(4-(tert-butoxycarbonylamino)-1H-indazol-1-yl)-2-(4-chlorophenyl)butanoate

생성물 1

HCID 705627322-(4-((tert-butoxycarbonyl)amino)-1H-indazol-1-yl)-2-(4-chlorophenyl)butanoic acid

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

반응 조건

온도
70 °C

실험 절차

Methyl 2-(4-((tert-butoxycarbonyl)amino)-1H-indazol-1-yl)-2-(4-chlorophenyl)butanoate (0.5 g, 1.13 mmol) (enantiomer A intermediate), as described in example 18 step D, as described in Example 18 step D, was dissolved in a mixture of 1,4-dioxane (1.0 mL) and water (0.25 mL) followed by addition of LiOH (0.27 g, 11.26 mmol). The mixture was stirred at 70° C. for 5 hours, then concentrated to remove solvent. The residue was dissolved in water (20 mL) and acidified with 1 N aq. HCl solution (11.3 mL) to give white precipitate. The solid was filtered, washed with water, and dried under vacuum to give title compound. LC/MS m/z=430.1[M+H]+.

후처리

  1. concentrationconcentrated
  2. customto remove solvent
  3. dissolutionThe residue was dissolved in water (20 mL)
  4. customto give white precipitate
  5. filtrationThe solid was filtered
  6. washwashed with water
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-91f7535e6a3b41f086823b6dff9eacbd
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403807B2

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