Dichloromethane → (E)-3-(2-Oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-6-yl)acrylic acid hydrochloride

HRID 83032

반응식

HRID 83032 반응식
FC(F)(F)C(O)=O.[O:8]=[C:9]1[NH:26][C:12]2=[N:13][CH:14]=[C:15](/[CH:17]=[CH:18]/[C:19]([O:21]C(C)(C)C)=[O:20])[CH:16]=[C:11]2[NH:10]1.[Cl:27]CCl>>[ClH:27].[O:8]=[C:9]1[NH:26][C:12]2=[N:13][CH:14]=[C:15](/[CH:17]=[CH:18]/[C:19]([OH:21])=[O:20])[CH:16]=[C:11]2[NH:10]1

참가 물질

4

실험 절차

Trifluoroacetic acid (2 mL) was added to a suspension of (E)-tert-butyl 3-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-6-yl)acrylate (400 mg, 1.54 mmol) in dichloromethane (2 mL) at room temperature. The reaction mixture was stirred for 1 hour then concentrated to dryness. The resulting residue was suspended in a solution of hydrochloric acid in dioxane 4N (2 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 (381 mg, quantitative).

후처리

  1. concentrationthen concentrated 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-8db42b6817374918a216ec71de8f61c2
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846711B2

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