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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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4-Chloro-2-(methylthio)pyrimidine-5-carboxylic acid ethyl ester → 8-Cyclopentyl-2-methylsulfanyl-5-oxo-5,6,7,8-tetrahydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

HRID 1989023
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HRID 1989023 반응식
[CH2:1]([O:3][C:4](=[O:13])[CH2:5][CH2:6][NH:7][CH:8]1[CH2:12][CH2:11][CH2:10][CH2:9]1)[CH3:2].C([O:16][C:17]([C:19]1[C:20](Cl)=[N:21][C:22]([S:25][CH3:26])=[N:23][CH:24]=1)=O)C.C(N(C(C)C)CC)(C)C>C(Cl)Cl>[CH2:1]([O:3][C:4]([CH:5]1[CH2:6][N:7]([CH:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)[C:20]2[N:21]=[C:22]([S:25][CH3:26])[N:23]=[CH:24][C:19]=2[C:17]1=[O:16])=[O:13])[CH3:2]
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참가 물질

5

반응물 3

HCID 800084-Chloro-2-(methylthio)pyrimidine-5-carboxylic acid ethyl esterHCID 81531DiisopropylethylamineHCID 23053028Ethyl 3-(cyclopentylamino)propanoate

생성물 1

HCID 686800598-Cyclopentyl-2-methylsulfanyl-5-oxo-5,6,7,8-tetrahydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Cyclopentylamino-propionic acid ethyl ester (1.0 g, 5.4 mmol) and 4-chloro-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester (1.25 g, 5.4 mmol) were combined in DCM (10 mL) and diisopropylethylamine (0.83 g, 6.5 mmol) was added. After 16 h, the solution was partitioned between water and DCM and the organic layer was dried (MgSO4) and concentrated. Chromatography (0-20% EtOAc/hexanes gradient) provided the title compound that was directly carried on to the next step. Sodium (25 wt % dispersion in paraffin wax, 0.25 g, 6.0 mmol) was added to t-butanol (5.0 mL) at rt. After 10 minutes, a solution of 4-[cyclopentyl-(2-ethoxycarbonyl-ethyl)-amino]-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester (2.0 g, 5.4 mmol) in 10 mL of toluene was added to the sodium t-butoxide solution and the resulting mixture was heated at 90° C. for 30 minutes. The reaction mixture was then cooled and the solution was adjusted to pH 7 using a 1N HCl solution. The solution was then extracted with EtOAc (2×20 mL) and the organic layer was dried (MgSO4) and concentrated to provide 0.26 g (14%). 1H-NMR (400 MHz, CDCl3:) 5 ppm 12.0 (br s, 1H), 8.20 (s, 1H), 5.10-5.18 (m, 1H), 4.26-4.31 (m, 3H), 3.72 (q, 2H, J=7.0 Hz), 2.50 (s, 3H), 1.63-1.86 (m, 5H), 1.20-1.35 (m, 5H).

후처리

  1. customthe solution was partitioned between water and DCM
  2. dry with materialthe organic layer was dried (MgSO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c765d6fab05e4d67a6d3b90188c23c76
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07642270B2

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