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

HRID 2172074

反応式

HRID 2172074 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-174deae5ff3f4441a4dbb605f82924c7
出典データセット
uspto-grants-2015_06
特許番号
US09051321B2

関連ノート

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