Hydrochloric Acid → 2-Fluoro-4-[3-(1-quinolin-6-ylcyclopropyl)[1,2,4]triazolo[4,3-b][1,2,4]triazin-6-yl]benzoic acid

HRID 2245993노트

반응식

HRID 2245993 반응식
[F:1][C:2]1[CH:11]=[C:10]([C:12]2[CH:13]=[N:14][C:15]3[N:16]([C:18]([C:21]4([C:24]5[CH:25]=[C:26]6[C:31](=[CH:32][CH:33]=5)[N:30]=[CH:29][CH:28]=[CH:27]6)[CH2:23][CH2:22]4)=[N:19][N:20]=3)[N:17]=2)[CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[OH-].[Li+].Cl>O1CCCC1.CO.O>[F:1][C:2]1[CH:11]=[C:10]([C:12]2[CH:13]=[N:14][C:15]3[N:16]([C:18]([C:21]4([C:24]5[CH:25]=[C:26]6[C:31](=[CH:32][CH:33]=5)[N:30]=[CH:29][CH:28]=[CH:27]6)[CH2:22][CH2:23]4)=[N:19][N:20]=3)[N:17]=2)[CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 59216283Methyl 2-fluoro-4-[3-(1-quinolin-6-ylcyclopropyl) [1,2,4]triazolo[4,3-b][1,2,4]triazin-6-yl]benzoate

생성물 1

HCID 592163392-Fluoro-4-[3-(1-quinolin-6-ylcyclopropyl)[1,2,4]triazolo[4,3-b][1,2,4]triazin-6-yl]benzoic acid수율 82.8%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

Methyl 2-fluoro-4-[3-(1-quinolin-6-ylcyclopropyl) [1,2,4]triazolo[4,3-b][1,2,4]triazin-6-yl]benzoate (0.15 g, 0.34 mmol) was dissolved in a solution of tetrahydrofuran (3 mL), methanol (1 mL) and water (1 mL) under N2 atmosphere. To the solution was added lithium hydroxide aqueous solution (2.0 M, 0.30 mL) with stirring. The mixture was stirred at RT for 1 h, and acidified with 1.0 M of hydrogen chloride in water (0.68 mL). The organic solvents were removed. The formed precipitate was collected by filtration, and dried in-vacuo to afford the desired product (120 mg). Analytical LCMS: (M+H)+=427.0.

후처리

  1. stirringThe mixture was stirred at RT for 1 h
  2. customThe organic solvents were removed
  3. filtrationThe formed precipitate was collected by filtration
  4. customdried in-vacuo

출처 및 근거

ORD 기록
ord-0a3b149fdc0f4f9a939eb5ac385cece7
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07683060B2

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