1-(3-Chlorophenyl)-3-(dimethylamino)-2-propen-1-one → 7-(3-Chlorophenyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile

HRID 231502ノート

反応式

HRID 231502 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8](=O)[CH:9]=[CH:10][N:11]([CH3:13])C)[CH:5]=[CH:6][CH:7]=1.N[C:16]1[C:20]([C:21]#[N:22])=C[NH:18][N:17]=1>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[N:18]3[N:17]=[CH:16][C:20]([C:21]#[N:22])=[C:13]3[N:11]=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 7300651-(3-Chlorophenyl)-3-(dimethylamino)-2-propen-1-oneHCID 178510443HCID 178510443、化合物

生成物 1

HCID 145018677-(3-Chlorophenyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile収率 83.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 50.0 g of 3'-chloro-3-dimethylaminoacrylophenone, 25.0 g of 3-aminopyrazole-4-carbonitrile and 500 ml of glacial acetic acid was heated at reflux for 2 hours. The mixture went into solution upon heating and a precipitate formed after one hour of refluxing. The reaction mixture was filtered and the crystals collected were triturated with saturated aqueous sodium bicarbonate, filtered and washed with water and then dried to give 49.0 g of the product of the example as colorless crystals, mp 238°-240° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. temperatureupon heating
  4. customa precipitate formed after one hour
  5. temperatureof refluxing
  6. filtrationThe reaction mixture was filtered
  7. customthe crystals collected
  8. customwere triturated with saturated aqueous sodium bicarbonate
  9. filtrationfiltered
  10. washwashed with water
  11. customdried

出典と根拠

ORDレコード
ord-22f74d8b701f46988c17a46b233e3e49
出典データセット
uspto-grants-1989_07
特許番号
US04847256

反応ノート

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