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

HRID 223416

반응식

HRID 223416 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-571d4729c84c4820b9fa50bf881db780
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04354031

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