Lithium hydroxide, monohydrate → 6-Fluoro-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylic acid

HRID 1802184노트

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HRID 1802184 반응식
[F:1][C:2]1[C:3]([C:17]([O:19]C)=[O:18])=[CH:4][C:5]2[N:6]([N:8]=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[N:10]=2)[CH:7]=1.O.[OH-].[Li+]>O1CCCC1.O>[F:1][C:2]1[C:3]([C:17]([OH:19])=[O:18])=[CH:4][C:5]2[N:6]([N:8]=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[N:10]=2)[CH:7]=1

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 67776717Methyl 6-fluoro-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylate

생성물 1

HCID 677761426-Fluoro-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylic acid수율 87.4%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

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온도
25 °C

실험 절차

A mixture of methyl 6-fluoro-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylate (600 mg, 2.21 mmol) and lithium hydroxide monohydrate (186 mg, 4.42 mmol) in tetrahydrofurane (10 ml) and water (2.0 ml) is stirred for 3 hours at 25° C. The solvent is evaporated, the residue diluted with water (ca 10 ml) and acidified with 2N aqueous hydrochloric acid (2.2 ml), the precipitated red solid is collected by filtration, washed with water and dried affording 6-fluoro-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylic acid (497 mg. 87.4%) as a pink solid. Mp.: >250° C. MS: m/z=329.2 (M−H+).

후처리

  1. customThe solvent is evaporated
  2. additionthe residue diluted with water (ca 10 ml)
  3. filtrationthe precipitated red solid is collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-d95b8057d3434cfe89fb35309b9c2907
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349824B2

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