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Phosphorus oxychloride → 7-Chloro-2-(methylthio)pyrido[2,3-d]pyrimidine

HRID 1826580
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반응식

HRID 1826580 반응식
[CH3:1][S:2][C:3]1[N:4]=[CH:5][C:6]2[CH:12]=[CH:11][C:10](=O)[NH:9][C:7]=2[N:8]=1.P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:10]1[CH:11]=[CH:12][C:6]2[CH:5]=[N:4][C:3]([S:2][CH3:1])=[N:8][C:7]=2[N:9]=1
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참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 12347632-(methylthio)pyrido(2,3-d)pyrimidin-7(8H)-one

생성물 1

HCID 221346737-Chloro-2-(methylthio)pyrido[2,3-d]pyrimidine

실험 절차

A suspension of 1.0 g (5.2 mmol) of 2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one (Example 5) in 10 mL of phosphorus oxychloride is heated under reflux for 1 hour. The resulting solution is cooled and concentrated to give a solid, which is triturated with cold water and filtered to give 1.05 g of crude product. Recrystallization from acetonitrile lives 0.76 g (69%) of the product, mp 201-203° C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 1 hour
  3. temperatureThe resulting solution is cooled
  4. concentrationconcentrated
  5. customto give a solid, which
  6. customis triturated with cold water
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-5263f83a165b4aa3bfa7ae1d7330fd57
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07053070B2

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