Phosphorus oxychloride → 3-(4-chloro-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-2-methylbenzonitrile

HRID 1098240노트

반응식

HRID 1098240 반응식
P(Cl)(Cl)([Cl:3])=O.O[C:7]1[N:12]=[CH:11][N:10]=[C:9]2[N:13]([C:16]3[C:17]([CH3:24])=[C:18]([CH:21]=[CH:22][CH:23]=3)[C:19]#[N:20])[N:14]=[CH:15][C:8]=12>>[Cl:3][C:7]1[N:12]=[CH:11][N:10]=[C:9]2[N:13]([C:16]3[C:17]([CH3:24])=[C:18]([CH:21]=[CH:22][CH:23]=3)[C:19]#[N:20])[N:14]=[CH:15][C:8]=12

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178428499HCID 178428499, 화합물

생성물 1

HCID 575046943-(4-chloro-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-2-methylbenzonitrile수율 86.1%

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온도
100 °C

실험 절차

Phosphoryl trichloride (9.92 ml, 103.49 mmol) was added to 3-(4-hydroxy-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-2-methylbenzonitrile (Intermediate AT3) (1.3 g, 5.17 mmol). The resulting solution was stirred at 100° C. for 2 hours. The reaction mixture was evaporated (azeotroping with toluene ×3) giving a brown oil which was triturated with ice/water to give afford the product (1.200 g) which was used without further purification.

후처리

  1. customThe reaction mixture was evaporated
  2. custom(azeotroping with toluene ×3)
  3. customgiving a brown oil which
  4. customwas triturated with ice/water
  5. customto give

출처 및 근거

ORD 기록
ord-a945f6c33f5649769e7272b6f37bde92
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143263B2

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