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

HRID 633986

反応式

HRID 633986 の反応式
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

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 68338066(E)-tert-butyl 3-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-6-yl)acrylate

生成物 1

HCID 70926863(E)-3-(2-Oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-6-yl)acrylic acid hydrochloride

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-c81b3737da8443f2a2fe7b8637210c0a
出典データセット
uspto-grants-2016_04
特許番号
US09321769B2

関連ノート

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