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HCID 53629213, 화합물 → HCID 53629214, 화합물

HRID 1924345
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HRID 1924345 반응식
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]2[N:9]=[C:10]([CH:12]3[CH2:14][CH2:13]3)[CH:11]=[C:4]2[N:3]=1>CC(O)=O.[Zn]>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]2[N:9]=[C:10]([CH:12]3[CH2:14][CH2:13]3)[CH:11]=[C:4]2[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 53629213HCID 53629213, 화합물

생성물 1

HCID 53629214HCID 53629214, 화합물수율 70%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

To a solution of 5,7-dichloro-2-cyclopropylpyrazolo[1,5-a]pyrimidine x272 (26.7 mmol, 1 eq., 6.08 g) in 125 ml of AcOH is added Zn powder (0.107 mol, 4 eq, 6.97 g). The mixture is then stirred for 48 hours at room temperature. After this time, the solvent is evaporated under reduce pressure and the reaction mixture poured on water, quenched with NaHCO3, and extracted with dichloromethane. The organic layer is dried over Na2SO4, filtered and evaporated under reduced pressure. The crude product is purified by chromatography on silicagel (CH2Cl2/hexane: 50/50) to afford 5-chloro-2-cyclopropylpyrazolo[1,5-a]pyrimidine x274 as a solid (3.60 g).

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후처리

  1. customAfter this time, the solvent is evaporated
  2. additionthe reaction mixture poured on water
  3. customquenched with NaHCO3
  4. extractionextracted with dichloromethane
  5. dry with materialThe organic layer is dried over Na2SO4
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customThe crude product is purified by chromatography on silicagel (CH2Cl2/hexane: 50/50)

출처 및 근거

ORD 기록
ord-59ba21fcf62348209ff5fa86d0b239bc
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178533B2

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