Acetic Anhydride → HCID 67973349, 화합물

HRID 623884노트

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HRID 623884 반응식
[C:1]([O:4]C(=O)C)(=[O:3])[CH3:2].[F:8][C:9]1[CH:10]=[C:11]([C:19]2[C:20]([CH3:34])=[CH:21][C:22]([O:25][CH2:26][C:27]([CH3:33])([CH3:32])[C:28]([O:30][CH3:31])=[O:29])=[N:23][CH:24]=2)[CH:12]=[CH:13][C:14]=1[C:15](=[NH:18])[NH:16]O>C(O)(=O)C>[C:1]([OH:4])(=[O:3])[CH3:2].[C:15]([C:14]1[CH:13]=[CH:12][C:11]([C:19]2[C:20]([CH3:34])=[CH:21][C:22]([O:25][CH2:26][C:27]([CH3:32])([CH3:33])[C:28]([O:30][CH3:31])=[O:29])=[N:23][CH:24]=2)=[CH:10][C:9]=1[F:8])(=[NH:16])[NH2:18]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 178500416HCID 178500416, 화합물

생성물 1

HCID 67973349HCID 67973349, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Acetic anhydride (1.62 mL) was added to an acetic acid (10 mL) solution containing methyl 3-({5-[3-fluoro-4-(N-hydroxycarbamimidoyl)phenyl]-4-methylpyridin-2-yl}-oxy)-2,2-dimethylpropanoate (3.65 g), and the mixture was stirred at room temperature for 5 hours. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in methanol (30 mL), 10% palladium carbon (50%, 365 mg) was added to the resulting solution, and the mixture was stirred under hydrogen atmosphere at room temperature for 13 hours. The catalyst was filtered off by using a membrane filter, and the filtrate was concentrated under reduced pressure. Ether was added to the obtained residue, and the precipitated solid was collected by filtration, washed with ether and dried to obtain methyl 3-{[5-(4-carbamimidoyl-3-fluorophenyl)-4-methylpyridin-2-yl]oxy}-2,2-dimethylpropanoate acetic acid salt (2.45 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in methanol (30 mL)
  3. addition10% palladium carbon (50%, 365 mg) was added to the resulting solution
  4. stirringthe mixture was stirred under hydrogen atmosphere at room temperature for 13 hours
  5. filtrationThe catalyst was filtered off
  6. filtrationfilter
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. additionEther was added to the obtained residue
  9. filtrationthe precipitated solid was collected by filtration
  10. washwashed with ether
  11. customdried

출처 및 근거

ORD 기록
ord-1415e56ea5d4457d9727dcbf662d8200
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302996B2

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