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

HRID 2300071
ノート
印刷プレビュー

反応式

HRID 2300071 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
175 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2e9eb46c89e047d49df879852f90ffc4
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06498163B1

反応ノート

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