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

HRID 883878노트

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HRID 883878 반응식
[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]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 86615483HCID 86615483, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid촉매

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온도
70 °C

실험 절차

The product from Example 21a (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%).

후처리

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

출처 및 근거

ORD 기록
ord-608ce14115fd44f48792e673871436d8
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08236950B2

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