Hydrazinecarbothioamide, N-phenyl- → 3-Anilino-4-acetyl-5-methylpyrazole

HRID 223416

反応式

HRID 223416 の反応式
[C:1]1([NH:7][C:8](=S)[NH:9][NH2:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:13][C:14]([CH2:16][C:17](=O)[CH3:18])=[O:15]>O1CCCC1>[NH:7]([C:8]1[C:16]([C:14](=[O:15])[CH3:13])=[C:17]([CH3:18])[NH:10][N:9]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 730679Hydrazinecarbothioamide, N-phenyl-HCID 144968561-Chloro-2,4-pentanedione

生成物 1

HCID 204753773-Anilino-4-acetyl-5-methylpyrazole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

50 g of 4-phenylthiosemicarbazide is suspended in 300 ml of tetrahydrofuran and 0.5 ml of concentrated HCL is added. Then 40.4 g of 3-chloroacetyl acetone is allowed to run in all at once and the whole is cooled with an ice-bath. After 12 hours' stirring, the precipitate formed is suction filtered, washed with acetone and then boiled in a water/acetone mixture (1:1). This hot solution is filtered off from the sulfur and neutralized with aqueous ammonia solution. The product is then suction filtered and recrystallized from acetone; m.p. 246°-247° C.

後処理

  1. addition0.5 ml of concentrated HCL is added
  2. temperatureis cooled with an ice-bath
  3. customthe precipitate formed
  4. filtrationfiltered
  5. washwashed with acetone
  6. filtrationThis hot solution is filtered off from the sulfur and neutralized with aqueous ammonia solution
  7. filtrationsuction filtered
  8. customrecrystallized from acetone

出典と根拠

ORDレコード
ord-571d4729c84c4820b9fa50bf881db780
出典データセット
uspto-grants-1982_10
特許番号
US04354031

関連ノート

読み込み中…