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

HRID 1695538
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HRID 1695538 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f79400d1096345099284a00214fc8a4b
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163742B2

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