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Hydrazine hydrate (1:1) → HCID 67083984, 화합물

HRID 79027
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HRID 79027 반응식
F[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([S:18][CH3:19])=[CH:14][C:13]=2[F:20])[C:3]=1[CH:21]=O.O.[NH2:24][NH2:25]>COCCOC>[F:20][C:13]1[CH:14]=[C:15]([S:18][CH3:19])[CH:16]=[CH:17][C:12]=1[NH:11][C:4]1[C:5]([C:6]([OH:8])=[O:7])=[CH:9][CH:10]=[C:2]2[C:3]=1[CH:21]=[N:24][NH:25]2
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 866562374-Fluoro-2-(2-fluoro-4-methylsulfanyl-phenylamino)-3-formyl-benzoic acid

생성물 1

HCID 67083984HCID 67083984, 화합물수율 82%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
90 °C

실험 절차

To a suspension of 4-fluoro-2-(2-fluoro-4-methylsulfanyl-phenylamino)-3-formyl-benzoic acid (105 mg, 0.32 mmol) in DME (5 mL) was added hydrazine hydrate (5 mL) and the reaction mixture heated at 90° C. for 18 hours. The volatile solvent was removed in vacuo and the residue acidified with concentrated HCl whilst applying cooling. The resultant precipitate was collected by filtration and washed with water to give the title compound as a tan solid (85 mg, 82%). LCMS (Method B) RT 3.12 [M+H]+ 318.

후처리

  1. customThe volatile solvent was removed in vacuo
  2. temperaturewhilst applying cooling
  3. filtrationThe resultant precipitate was collected by filtration
  4. washwashed with water

출처 및 근거

ORD 기록
ord-0fdb007c69104fa0a5cb5b6cc2588bbd
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841462B2

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