Dichloromethane → (E)-3-(3-ethoxycarbonylmethyl-2-oxo-1,2,3,4-tetrahydro-pyrido[2,3-d]pyrimidin-6-yl)acrylic acid hydrochloride

HRID 633973

反応式

HRID 633973 の反応式
FC(F)(F)C(O)=O.[CH2:8]([O:10][C:11](=[O:33])[CH2:12][N:13]1[CH2:18][C:17]2[CH:19]=[C:20](/[CH:23]=[CH:24]/[C:25]([O:27]C(C)(C)C)=[O:26])[CH:21]=[N:22][C:16]=2[NH:15][C:14]1=[O:32])[CH3:9].[Cl:34]CCl>>[ClH:34].[CH2:8]([O:10][C:11](=[O:33])[CH2:12][N:13]1[CH2:18][C:17]2[CH:19]=[C:20](/[CH:23]=[CH:24]/[C:25]([OH:27])=[O:26])[CH:21]=[N:22][C:16]=2[NH:15][C:14]1=[O:32])[CH3:9]

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 66967516(E)-tert-Butyl 3-(3-(2-ethoxy-2-oxoethyl)-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidin-6-yl)acrylate

生成物 1

HCID 66966906(E)-3-(3-ethoxycarbonylmethyl-2-oxo-1,2,3,4-tetrahydro-pyrido[2,3-d]pyrimidin-6-yl)acrylic acid hydrochloride

実験手順

Trifluoroacetic acid (5 mL) was added to a solution of (E)-tert-butyl 3-(3-(2-ethoxy-2-oxoethyl)-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidin-6-yl)acrylate (460 mg, 1.27 mmol) in dichloromethane (5 mL) at room temperature. The reaction mixture was stirred at room temperature for 30 minutes. After concentration to dryness, the residue was suspended in a solution of hydrochloric acid in dioxane 4N (10 mL). The resulting white precipitate was filtered and washed with diethyl ether to give the title compound (470 mg; quantitative).

後処理

  1. concentrationAfter concentration to dryness
  2. filtrationThe resulting white precipitate was filtered
  3. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-eb7814257e6842c2a9f3685dfd241130
出典データセット
uspto-grants-2016_04
特許番号
US09321769B2

関連ノート

読み込み中…