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Sodium Hydroxide → (2-(5-Fluoro-2-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetic acid

HRID 1372645
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반응식

HRID 1372645 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:24])=[C:6]([NH:8][C:9]2[O:10][C:11]3[C:17]([F:18])=[C:16]([CH2:19][C:20]([O:22]C)=[O:21])[CH:15]=[CH:14][C:12]=3[N:13]=2)[CH:7]=1.[OH-].[Na+]>C1COCC1.CO>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:24])=[C:6]([NH:8][C:9]2[O:10][C:11]3[C:17]([F:18])=[C:16]([CH2:19][C:20]([OH:22])=[O:21])[CH:15]=[CH:14][C:12]=3[N:13]=2)[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 44607521Methyl (2-(5-fluoro-2-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetate

생성물 1

HCID 17858947(2-(5-Fluoro-2-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetic acid수율 90.1%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

In THF/methanol (2:1, v/v, 90 ml) was dissolved methyl (2-(5-fluoro-2-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetate (810 mg, 2.44 mmol). To the resulting solution was added 1N NaOH (30 ml). After stirring at room temperature for 12 hours, the reaction mixture was distilled under reduced pressure to remove the solvent. The residue was acidified with 1N HCl. The crystals thus precipitated were collected by filtration under reduced pressure, washed with water and dried under reduced pressure to give (2-(5-fluoro-2-methylphenylamino)-7-fluoro-6-benzoxazolyl)acetic acid (700 mg, 90%) as a pale brown solid.

후처리

  1. distillationthe reaction mixture was distilled under reduced pressure
  2. customto remove the solvent
  3. customThe crystals thus precipitated
  4. filtrationwere collected by filtration under reduced pressure
  5. washwashed with water
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-bf50028ecab84df4b253bb15e02d7471
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157487B2

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