HCID 57743058、化合物 → HCID 57743030、化合物

HRID 1896420ノート

反応式

HRID 1896420 の反応式
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

参加物

4

反応物 1

HCID 57743058HCID 57743058、化合物

生成物 1

HCID 57743030HCID 57743030、化合物収率 90%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-952d6ec651984b039d74ffbe6b3fdfe1
出典データセット
uspto-grants-2013_08
特許番号
US08518943B2

反応ノート

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