Sulfuric Acid → Ethyl 7-chloro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate

HRID 2197726ノート

反応式

HRID 2197726 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[N:10][C:11]([Cl:17])=[CH:12][CH:13]=2)[N:8](C(C)(C)C)[CH:7]=1)=[O:5])[CH3:2].S(=O)(=O)(O)O>C(O)(C(F)(F)F)=O>[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[N:10][C:11]([Cl:17])=[CH:12][CH:13]=2)[NH:8][CH:7]=1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 86615483HCID 86615483、化合物

生成物 1

HCID 12804018Ethyl 7-chloro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate収率 93.1%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid触媒

反応条件

温度
70 °C

実験手順

The product from Example 13a (0.282 gm, 0.91 mmol) was combined at room temperature with 2 mL of TFA containing 2 drops of sulfuric acid. The resulting mixture was heated at 70° C. for 16.5 h. The volatiles were removed under vacuum and the residue suspended in water. The product was collected by vacuum filtration, water washed and dried under vacuum to give the title compound as a cream colored solid (0.214 gm, 93%).

後処理

  1. customThe volatiles were removed under vacuum
  2. filtrationThe product was collected by vacuum filtration, water
  3. washwashed
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-da366b1440fa4dc5b9ee2475d2d6c28f
出典データセット
uspto-grants-2012_12
特許番号
US08338605B2

反応ノート

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