Lithium hydroxide, monohydrate → HCID 59587418, 화합물

HRID 1410433노트

반응식

HRID 1410433 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[O:10][C:11]([C:22]([O:24]CC)=[O:23])=[C:12]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[N:13]=1.O.[OH-].[Li+]>C1COCC1.O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[O:10][C:11]([C:22]([OH:24])=[O:23])=[C:12]([C:14]2[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=2)[N:13]=1

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 59587539HCID 59587539, 화합물

생성물 1

HCID 59587418HCID 59587418, 화합물수율 100%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of ethyl 2-(2,6-difluorophenyl)-4-(4-methoxyphenyl)oxazole-5-carboxylate (0.030 g, 0.08 mmol) in THF and H2O (1:1, 3 mL) was added lithium hydroxide hydrate (0.008 g, 0.33 mmol) and the reaction mixture stirred at room temperature for 2.5 hours. The THF was removed in vacuo and 1N aqueous HCl was added and the resultant precipitate collected by filtration to afford 2-(2,6-difluorophenyl)-4-(4-methoxyphenyl)oxazole-5-carboxylic acid (0.027 g, 0.08 mmol, 98%) as a white solid which was used without further purification. LCMS (1) Rt: 1.24 min; m/z (ES+) 332.

후처리

  1. customThe THF was removed in vacuo and 1N aqueous HCl
  2. additionwas added
  3. filtrationthe resultant precipitate collected by filtration

출처 및 근거

ORD 기록
ord-88a0ad77ef824539bc5608f88daf1da3
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921544B2

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