Lithium hydroxide, monohydrate → HCID 59587418、化合物

HRID 389700ノート

反応式

HRID 389700 の反応式
[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

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 59587539HCID 59587539、化合物

生成物 1

HCID 59587418HCID 59587418、化合物収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4e8790cceab84b5c8303c256b5787b42
出典データセット
uspto-grants-2013_02
特許番号
US08378095B2

反応ノート

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