Dichloromethane → (E)-3-(7-oxo-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)acrylic Acid Hydrochloride

HRID 82902

반응식

HRID 82902 반응식
FC(F)(F)C(O)=O.[O:8]=[C:9]1[NH:18][C:17]2[N:16]=[CH:15][C:14](/[CH:19]=[CH:20]/[C:21]([O:23]C(C)(C)C)=[O:22])=[CH:13][C:12]=2[CH2:11][CH2:10]1.[Cl:28]CCl>>[ClH:28].[O:8]=[C:9]1[NH:18][C:17]2[N:16]=[CH:15][C:14](/[CH:19]=[CH:20]/[C:21]([OH:23])=[O:22])=[CH:13][C:12]=2[CH2:11][CH2:10]1

참가 물질

4

실험 절차

Trifluoroacetic acid (31 mL) was added to a suspension of tert-butyl (E)-3-(7-Oxo-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)-acrylate (1.1 g, 3.76 mmol; which may be prepared as described in D1, Step 6) in dichloromethane (31 mL). The reaction mixture was stirred at room temperature for 1 hour and concentrated to dryness. The resulting residue was solubilized in a solution of hydrochloric acid in dioxane (4N, 60 mL). After 10 minutes stirring at room temperature, the precipitate was filtered and washed with diethyl ether to afford the title product as a pale yellow solid (4.5 g, quantitative).

후처리

  1. concentrationconcentrated to dryness
  2. stirringAfter 10 minutes stirring at room temperature
  3. filtrationthe precipitate was filtered
  4. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-de4a329500ce4915a5dda5f1cb0ac9ce
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846711B2

연결된 노트

불러오는 중…