Methanol → HCID 178493687, 화합물

HRID 930452노트

반응식

HRID 930452 반응식
Cl[C:2]1[CH:11]=[N:10][C:9]2[C:8](=[O:12])[N:7]=[CH:6][NH:5][C:4]=2[CH:3]=1.[CH3:13][O-:14].[Na+].CO.[Cl-].[NH4+]>>[CH3:13][O:14][C:2]1[CH:11]=[N:10][C:9]2[C:8](=[O:12])[N:7]=[CH:6][NH:5][C:4]=2[CH:3]=1

참가 물질

5

반응물 4

HCID 887MethanolHCID 25517Ammonium ChlorideHCID 10942334Sodium Methoxide2회HCID 1785182197-chloro-1H-pyrido[3,2-d]pyrimidin-4-one

생성물 1

HCID 178493687HCID 178493687, 화합물

실험 절차

A microwave vial was charged with 7-chloropyrido[3,2-d]pyrimidin-4(1H)-one (110 mg, 0.606 mmol), a 0.5 M solution of sodium methoxide in methanol (3.65 mL, 1.817 mmol) and sodium methoxide (327 mg, 6.06 mmol). The vial was capped and irradiated in a microwave reactor at 145° C. for 30 minutes. The reaction was neutralized with saturated aqueous ammonium chloride (3 mL), concentrated, and diluted with cold water. The resulting precipitate was collected by vacuum filtration and dried in vacuo to provide the title compound (107 mg, 0.604 mmol) as pink solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 3.95 (s, 3 H) 7.49 (d, J=2.74 Hz, 1 H) 8.11 (s, 1 H) 8.47 (d, J=2.74 Hz, 1 H). LC/MS (ESI+) m/z=178 (M+H).

후처리

  1. customThe vial was capped
  2. customirradiated in a microwave reactor at 145° C. for 30 minutes
  3. concentrationconcentrated
  4. additiondiluted with cold water
  5. filtrationThe resulting precipitate was collected by vacuum filtration
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-aeda161efce34c1289ae93cf0a4107e2
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296734B2

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