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

HRID 1851190노트

반응식

HRID 1851190 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 were stirred for 3 h at 50° C. The mixture was filtered through celite, evaporated to dryness and the residue was 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 was filtered through celite
  2. customevaporated to dryness
  3. customthe residue was purified on silica gel (hexanes/ethyl acetate)
  4. customto yield

출처 및 근거

ORD 기록
ord-b4d00eedd7ab447eb3b1f032aabe153a
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957064B2

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