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

HRID 82902
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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
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참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 10869488tert-butyl (E)-3-(7-oxo-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)acrylate

생성물 1

HCID 66905305(E)-3-(7-oxo-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)acrylic Acid Hydrochloride

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
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846711B2

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