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

HRID 1851190ノート

反応式

HRID 1851190 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b4d00eedd7ab447eb3b1f032aabe153a
出典データセット
uspto-grants-2015_02
特許番号
US08957064B2

反応ノート

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