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Sodium Hydroxide → HCID 86691785, 화합물

HRID 1500767
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HRID 1500767 반응식
[N:1]1[N:5]2[CH:6]=[CH:7][N:8]=[CH:9][C:4]2=[C:3]([C:10]2[N:15]=[C:14](O)[CH:13]=[CH:12][N:11]=2)[CH:2]=1.P(Cl)(Cl)([Cl:19])=O.[OH-].[Na+]>C(OCC)(=O)C>[Cl:19][C:14]1[CH:13]=[CH:12][N:11]=[C:10]([C:3]2[CH:2]=[N:1][N:5]3[CH:6]=[CH:7][N:8]=[CH:9][C:4]=23)[N:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 1785164942-(Pyrazolo[1,5-a]pyrazin-3-yl)pyrimidin-4-ol

생성물 1

HCID 86691785HCID 86691785, 화합물수율 104.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A solution of 2-(pyrazolo[1,5-a]pyrazin-3-yl)pyrimidin-4-ol (Preparation 10b, 150 mg, 0.7 mmol) in phosphorous oxychloride (1.42 mL, 15.51 mmol) was heated overnight at 110° C. After cooling to ambient temperature, the reaction mixture was poured with caution onto water and basified by addition of a 2N aqueous sodium hydroxide solution. Ethyl acetate was then added and the organic phase was separated, washed with water and brine, dried (MgSO4), filtered and evaporated under reduced pressure to yield the title compound (170 mg, 87%) as a solid which was used in the next synthetic step without further purification.

후처리

  1. additionthe reaction mixture was poured with caution onto water
  2. customthe organic phase was separated
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-53b0bd57eddd440b8d5e1affed9440a3
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206183B2

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