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

HRID 1915546ノート

反応式

HRID 1915546 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 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.

後処理

  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

出典と根拠

ORDレコード
ord-4449321a44404b87807073699c9f4a98
出典データセット
uspto-grants-2013_12
特許番号
US08614218B2

反応ノート

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