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Benzenamine, 4-(4-morpholinyl)- → C2 Pyrido[2,3-d]pyrimidin-7-one deriv. 34

HRID 2300071
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HRID 2300071 반응식
[CH2:1]([N:3]1[C:8]2[N:9]=[C:10](S(C)=O)[N:11]=[CH:12][C:7]=2[CH:6]=[CH:5][C:4]1=[O:16])[CH3:2].[O:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:29]=[CH:28][C:26]([NH2:27])=[CH:25][CH:24]=2)[CH2:19][CH2:18]1>C(OCC)(=O)C>[CH2:1]([N:3]1[C:8]2[N:9]=[C:10]([NH:27][C:26]3[CH:25]=[CH:24][C:23]([N:20]4[CH2:21][CH2:22][O:17][CH2:18][CH2:19]4)=[CH:29][CH:28]=3)[N:11]=[CH:12][C:7]=2[CH:6]=[CH:5][C:4]1=[O:16])[CH3:2]
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참가 물질

4

반응물 2

HCID 75655Benzenamine, 4-(4-morpholinyl)-HCID 10752351Pyrido[2,3-d]pyrimidin-7(8H)-one, 8-ethyl-2-(methylsulfinyl)-

생성물 1

HCID 5330220C2 Pyrido[2,3-d]pyrimidin-7-one deriv. 34

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
175 °C

실험 절차

A mixture of 8-ethyl-2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one (136 mg, 0.57 mmol) and 4-morpholinoaniline (205 mg, 1.15 mmol) was heated at 175° C. for 10 minutes then cooled to room temperature, and ethyl acetate was added. The precipitate was collected by filtration and purified by flash chromatography eluting with ethyl acetate. The fractions containing product were concentrated, and ethyl acetate and hexane were added to the residue. The resultant precipitate was collected by filtration to give 114 mg (57%) yield of 8-ethyl-2-(4-morpholin-4-yl-phenylamino)-8H-pyrido[2,3-d]pyrimidin-7-one, mp 227-228° C.

후처리

  1. temperaturethen cooled to room temperature
  2. filtrationThe precipitate was collected by filtration
  3. custompurified by flash chromatography
  4. washeluting with ethyl acetate
  5. additionThe fractions containing product
  6. concentrationwere concentrated
  7. additionethyl acetate and hexane were added to the residue
  8. filtrationThe resultant precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-2e9eb46c89e047d49df879852f90ffc4
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06498163B1

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