Hydrochloric Acid → 1-(2,4,6-Trichlorophenyl)-2-acetyl-3-(2-chloro-5-myristoylaminoanilino)-3-pyrazolin-5-one

HRID 460736노트

반응식

HRID 460736 반응식
N1C(C)=CC=CC=1C.[Cl:9][C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([Cl:17])[C:11]=1[N:18]1[C:22](=[O:23])[CH2:21][C:20]([NH:24][C:25]2[CH:30]=[C:29]([NH:31][C:32](=[O:46])[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])[CH:28]=[CH:27][C:26]=2[Cl:47])=[N:19]1.[Cl-].[Al+3].[Cl-].[Cl-].[C:52](Cl)(=[O:54])[CH3:53].Cl>ClCCl>[Cl:17][C:12]1[CH:13]=[C:14]([Cl:16])[CH:15]=[C:10]([Cl:9])[C:11]=1[N:18]1[C:22](=[O:23])[CH:21]=[C:20]([NH:24][C:25]2[CH:30]=[C:29]([NH:31][C:32](=[O:46])[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])[CH:28]=[CH:27][C:26]=2[Cl:47])[N:19]1[C:52](=[O:54])[CH3:53]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 79372,6-Lutidine2회HCID 6451240Aluminum(III) ChlorideHCID 178443172N-[4-chloro-3-[[5-oxo-1-(2,4,6-trichlorophenyl)-4H-pyrazol-3-yl]amino]phenyl]tetradecanamide

생성물 1

HCID 213940501-(2,4,6-Trichlorophenyl)-2-acetyl-3-(2-chloro-5-myristoylaminoanilino)-3-pyrazolin-5-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
10 °C

실험 절차

1.07 g (0.01 mole) of lutidine is added to a solution of 30.7 g (0.05 mole) of 1-(2,4,6-trichlorophenyl)-3-(2-chloro-5-myristoylaminoanilino)-2-pyrazolin-5-one and 8 g (0.06 mole) of anhydrous aluminium chloride in 100 ml of dichloromethane. The solution is cooled to 10° C and 5.90 g (0.075 mole) of acetylchloride are added. 8 g (0.075 mole) of lutidine divided into 4 portions of 2 g each (one portion every 15 min) are added in a total period of time of 1 h, the temperature being kept below 10° C. The reaction mixture is stirred for 2 h more and then poured out into 1 l of 1N aqueous hydrochloric acid. The dichloromethane layer is washed until free from acid, dried, and concentrated by evaporation. The product is agitated with methanol.

후처리

  1. customevery 15 min
  2. additionare added in a total period of time of 1 h
  3. custombeing kept below 10° C
  4. washThe dichloromethane layer is washed until free from acid
  5. customdried
  6. concentrationconcentrated by evaporation
  7. stirringThe product is agitated with methanol

출처 및 근거

ORD 기록
ord-1e047ed0942046248435f195249898c6
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061498

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