Methanol → HCID 178493687、化合物

HRID 930452ノート

反応式

HRID 930452 の反応式
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

参加物

5

反応物 4

HCID 887MethanolHCID 25517Ammonium ChlorideHCID 10942334Sodium Methoxide2 回HCID 1785182197-chloro-1H-pyrido[3,2-d]pyrimidin-4-one

生成物 1

HCID 178493687HCID 178493687、化合物

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-aeda161efce34c1289ae93cf0a4107e2
出典データセット
uspto-grants-2016_03
特許番号
US09296734B2

反応ノート

読み込み中…