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Water → HCID 59811153, 화합물

HRID 1724838
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HRID 1724838 반응식
[F:1][C:2]([F:38])([F:37])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]2[C:19]3[C:14](=[N:15][C:16]([C:20]4[C:25]([C:26]([F:29])([F:28])[F:27])=[CH:24][CH:23]=[CH:22][N:21]=4)=[CH:17][CH:18]=3)[N:13]=[C:12]([CH2:30][O:31][CH3:32])[C:11]=2[C:33]([O:35]C)=[O:34])=[CH:5][CH:4]=1.O[Li].O.C1COCC1.O>C(O)(=O)C>[F:38][C:2]([F:1])([F:37])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]2[C:19]3[C:14](=[N:15][C:16]([C:20]4[C:25]([C:26]([F:28])([F:29])[F:27])=[CH:24][CH:23]=[CH:22][N:21]=4)=[CH:17][CH:18]=3)[N:13]=[C:12]([CH2:30][O:31][CH3:32])[C:11]=2[C:33]([OH:35])=[O:34])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 59811134HCID 59811134, 화합물

생성물 1

HCID 59811153HCID 59811153, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Stir a solution of methyl 4-[(4-trifluoromethylphenyl)amino]-7-(3-trifluoromethylpyridin-2-yl)-2-methoxymethyl-[1,8]naphthyridine-3-carboxylate (114 mg, 0.212 mmol), LiOH.H2O (45.0 mg, 1.06 mmol), THF (2 mL) and water (0.1 mL) for 18 hours at room temperature. Add water (20 mL) and acidify with acetic acid. Extract the solution with EtOAc (3×25 mL). Wash the combined organic extracts with brine and dry over Na2SO4. Remove the solvent under reduced pressure to yield the title compound. MS 523.18 (M+1). 1H NMR δ (CDCl3) 11.50 (1H, br s), 8.89 (1H, s), 8.19 (2H, d), 7.88 (1H, dd), 7.67 (2H, m), 7.59 (1H, dd), 7.51 (2H, d), 7.22 (1H, br s), 5.30 (2H, s), 3.65 (3H, s).

후처리

  1. extractionExtract the solution with EtOAc (3×25 mL)
  2. washWash the combined organic extracts with brine
  3. dry with materialdry over Na2SO4
  4. customRemove the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-a35ed46437be431aa522a190321e87bd
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07488740B2

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