Lithium hydroxide, monohydrate → HCID 59587418、化合物

HRID 714933ノート

反応式

HRID 714933 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-cac2051453c74bd3964c708fa763e763
出典データセット
uspto-grants-2015_11
特許番号
US09187465B2

反応ノート

読み込み中…