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Sodium Hydroxide → HCID 9869853, 화합물

HRID 1368904
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HRID 1368904 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH:8][CH2:9][CH2:10][CH2:11][C:12]([NH:14][CH2:15][C:16]([NH:18][CH:19]([C:25]2[CH:30]=[CH:29][C:28]([O:31][C:32]([F:35])([F:34])[F:33])=[CH:27][CH:26]=2)[CH2:20][C:21]([O:23]C)=[O:22])=[O:17])=[O:13])[CH:3]=1.[OH-].[Na+]>O1CCOCC1>[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH:8][CH2:9][CH2:10][CH2:11][C:12]([NH:14][CH2:15][C:16]([NH:18][CH:19]([C:25]2[CH:26]=[CH:27][C:28]([O:31][C:32]([F:35])([F:34])[F:33])=[CH:29][CH:30]=2)[CH2:20][C:21]([OH:23])=[O:22])=[O:17])=[O:13])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 11294904HCID 11294904, 화합물

생성물 1

HCID 9869853HCID 9869853, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

280 mg of methyl 3-{2-[4-(4-methylpyridin-2-ylamino)butyrylamino]acetylamino}-3-(4-trifluoromethoxyphenyl)propionate (crude material) are dissolved in 30 ml of dioxane, and 0.61 ml of NaOH (2 mol/l) is added. Stirring at room temperature overnight is followed by removal of the solvent by distillation and the usual workup. 3-{2-[4-(4-methylpyridin-2-ylamino)butyrylamino]acetylamino}-3-(4-trifluoromethoxyphenyl)propionic acid is obtained. If an excess of NaOH is used, the sodium salt of 3-{2-[4-(4-methylpyridin-2-ylamino)butyrylamino]acetylamino}-3-(4-trifluoromethoxyphenyl)propionic acid is obtained. Preparative HPLC results in 3-{2-[4-(4-methylpyridin-2-ylamino)butyrylamino]acetylamino}-3-(4-trifluoromethoxyphenyl)propionic acid trifluoroacetate, RT 24.93 min, FAB-MS (M+H)+ 483.

후처리

  1. customis followed by removal of the solvent by distillation

출처 및 근거

ORD 기록
ord-02584d82b0b64921872dee1ba0066513
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06576637B1

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