HCID 57743058, 화합물 → HCID 57743030, 화합물

HRID 1896420노트

반응식

HRID 1896420 반응식
Cl[C:2]1[N:7]2[N:8]=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH:10]=[C:6]2[N:5]=[C:4]([CH3:17])[C:3]=1[F:18]>CC(O)=O.[Zn]>[F:18][C:3]1[C:4]([CH3:17])=[N:5][C:6]2[N:7]([N:8]=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH:10]=2)[CH:2]=1

참가 물질

4

반응물 1

HCID 57743058HCID 57743058, 화합물

생성물 1

HCID 57743030HCID 57743030, 화합물수율 90%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

반응 조건

온도
25 °C

실험 절차

To a solution of 7-chloro-6-fluoro-5-methyl-2-phenylpyrazolo[1,5-a]pyrimidine x136 (22.9 mmol, 1 eq, 6 g) in 150 ml of AcOH at 0° C., is added zinc dust (68 mmol, 3 eq, 4.5 g). The mixture is stirred at 25° C. overnight. After evaporation of the solvent under reduced pressure, the crude product is poured on ice and quenched with a saturated aqueous NaHCO3 solution and extracted with AcOEt. The cumulated organic layers are washed with brine, dried over MgSO4, filtered and evaporated under reduced pressure to yield 6-fluoro-5-methyl-2-phenylpyrazolo[1,5-a]pyrimidine x139.

후처리

  1. customAfter evaporation of the solvent under reduced pressure
  2. additionthe crude product is poured on ice
  3. customquenched with a saturated aqueous NaHCO3 solution
  4. extractionextracted with AcOEt
  5. washThe cumulated organic layers are washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-952d6ec651984b039d74ffbe6b3fdfe1
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518943B2

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