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

HRID 2172074

반응식

HRID 2172074 반응식
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]

참가 물질

4

반응물 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

생성물 1

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

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-174deae5ff3f4441a4dbb605f82924c7
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051321B2

연결된 노트

불러오는 중…