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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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N-(3-Aminopropyl)morpholine → 6-(2,6-dichlorophenyl)-8-methyl-2-{[3-(morpholin-4-yl)propyl]amino}-7H,8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3188
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인쇄 미리보기

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HRID 3188 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:20](=[O:21])[N:19]([CH3:22])[C:12]2[N:13]=[C:14](SC)[N:15]=[CH:16][C:11]=2[CH:10]=1.[NH2:23][CH2:24][CH2:25][CH2:26][N:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:20](=[O:21])[N:19]([CH3:22])[C:12]2[N:13]=[C:14]([NH:23][CH2:24][CH2:25][CH2:26][N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)[N:15]=[CH:16][C:11]=2[CH:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 61055N-(3-Aminopropyl)morpholineHCID 107367016-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one

생성물 1

HCID 53278776-(2,6-dichlorophenyl)-8-methyl-2-{[3-(morpholin-4-yl)propyl]amino}-7H,8H-pyrido[2,3-d]pyrimidin-7-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
125 °C

실험 절차

A mixture of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 1.00 g (6.90 mmol) of N-(3-aminopropyl)morpholine and 0.5 mL of dimethylformamide was heated with stirring in a 125° C. oil bath. After 2 minutes, solution was complete. After 1.5 hours, the excess amine and dimethylformamide were evaporated at reduced pressure and the residue was triturated with 5 mL of water. The gum was dissolved in 25 mL of ethyl acetate, and the solution was washed with 2×5 mL of water, dried (potassium carbonate), and concentrated. Upon dissolution in 5 mL of ether, crystals of pure product separated; wt 0.101 g; mp 140°-142° C.

후처리

  1. temperaturewas heated
  2. waitAfter 1.5 hours
  3. customthe excess amine and dimethylformamide were evaporated at reduced pressure
  4. customthe residue was triturated with 5 mL of water
  5. dissolutionThe gum was dissolved in 25 mL of ethyl acetate
  6. washthe solution was washed with 2×5 mL of water
  7. dry with materialdried (potassium carbonate)
  8. concentrationconcentrated
  9. dissolutionUpon dissolution in 5 mL of ether
  10. customcrystals of pure product separated

출처 및 근거

ORD 기록
ord-ed41f375aaff41018a80d7b0ecb415a0
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05733914

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