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Lithium Hydroxide → 6-Chloro-3-(3-(trifluoromethyl)phenylamino)benzo[d]isoxazole-7-carboxylic acid

HRID 1695538
ノート
印刷プレビュー

反応式

HRID 1695538 の反応式
[Cl:1][C:2]1[CH:21]=[CH:20][C:5]2[C:6]([NH:9][C:10]3[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=3)=[N:7][O:8][C:4]=2[C:3]=1[C:22]([O:24]C)=[O:23].[Li+].[OH-]>O1CCOCC1>[Cl:1][C:2]1[CH:21]=[CH:20][C:5]2[C:6]([NH:9][C:10]3[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:18])([F:17])[F:19])[CH:11]=3)=[N:7][O:8][C:4]=2[C:3]=1[C:22]([OH:24])=[O:23]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 67276645Methyl 6-chloro-3-(3-(trifluoromethyl)phenylamino)benzo[d]isoxazole-7-carboxylate

生成物 1

HCID 441404356-Chloro-3-(3-(trifluoromethyl)phenylamino)benzo[d]isoxazole-7-carboxylic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
50 °C

実験手順

To a solution of methyl 6-chloro-3-(3-(trifluoromethyl)phenylamino)benzo[d]isoxazole-7-carboxylate (1.0 g, 2.8 mmol) in dioxane (30 mL) was added a 1N solution of LiOH, monohydrate (0.59 g, 14 mmol). The reaction mixture was heated at 50° C. for 2 h. The solvent was removed and to the aqueous solution was added 2N HCl until pH 4. The precipitate formed was collected by filtration, washed with water (5 mL) and dried to give 6-chloro-3-(3-(trifluoromethyl)phenylamino)benzo[d]isoxazole-7-carboxylic acid as off-white solid.

後処理

  1. customThe solvent was removed and to the aqueous solution
  2. additionwas added 2N HCl until pH 4
  3. customThe precipitate formed
  4. filtrationwas collected by filtration
  5. washwashed with water (5 mL)
  6. customdried

出典と根拠

ORDレコード
ord-f79400d1096345099284a00214fc8a4b
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163742B2

反応ノート

読み込み中…

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