Acetic Acid → 5-Chloro-6-phenylpyrazolo[1,5-a]pyrimidine

HRID 1915546노트

반응식

HRID 1915546 반응식
[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:6](Cl)[N:5]2[N:15]=[CH:16][CH:17]=[C:4]2[N:3]=1.C(O)(=O)C.CO>C1COCC1>[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:6][N:5]2[N:15]=[CH:16][CH:17]=[C:4]2[N:3]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 887MethanolHCID 594278075,7-Dichloro-6-phenylpyrazolo[1,5-a]pyrimidine

생성물 1

HCID 866306645-Chloro-6-phenylpyrazolo[1,5-a]pyrimidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

A mixture of 1 g 5,7-dichloro-6-phenylpyrazolo[1,5-a]pyrimidine, 0.5 ml glacial acetic acid, 1 ml methanol, 6 ml THF and 730 mg of Zn/Cu pair are stirred for 3 h at 50° C. The mixture is filtered through celite, evaporated to dryness and the residue is purified on silica gel (hexanes/ethyl acetate) to yield 550 mg of a 1:1 mixture of the desired product and the starting material, which was used without further purification.

후처리

  1. filtrationThe mixture is filtered through celite
  2. customevaporated to dryness
  3. customthe residue is purified on silica gel (hexanes/ethyl acetate)
  4. customto yield

출처 및 근거

ORD 기록
ord-4449321a44404b87807073699c9f4a98
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614218B2

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