Phosphorus oxychloride → HCID 178434472, 화합물

HRID 2426104노트

반응식

HRID 2426104 반응식
[CH3:1][C:2]1[N:3]=[N:4][C:5]2[C:10]=1[C:9](=O)[N:8]=[CH:7][N:6]=2.C(N(C(C)C)CC)(C)C.P(Cl)(Cl)([Cl:23])=O>>[Cl:23][C:9]1[N:8]=[CH:7][N:6]=[C:5]2[NH:4][N:3]=[C:2]([CH3:1])[C:10]=12

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 536298293-Methyl-pyrazolo[3,4-d]pyrimidin-4-one

생성물 1

HCID 178434472HCID 178434472, 화합물

실험 절차

To a stirred suspension of 3-methyl-pyrazolo[3,4-d]pyrimidin-4-one (7.50 g, 50.0 mmol, Example 2) in phosphorus oxychloride (150 mL) was added diisopropylethylamine (31 mL, 175 mmol, Aldrich). The mixture was heated at reflux for 2.5 hours before the solvent was evaporated under reduced pressure. The residue was treated with ice (200 g) and made slightly basic with 4N aqueous sodium hydroxide solution and extracted with ethyl acetate (3×250 mL). The combined organic extracts were washed with water, brine, dried and concentrated to give 4-chloro-3-methyl-1H-pyrazolo[3,4-d]pyrimidine as a white solid. (Yield 6.38 g).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 2.5 hours before the solvent
  3. customwas evaporated under reduced pressure
  4. additionThe residue was treated with ice (200 g)
  5. extractionextracted with ethyl acetate (3×250 mL)
  6. washThe combined organic extracts were washed with water, brine
  7. customdried
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-72a0ea1cac81476683bb0a59f1c84677
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968554B2

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