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

HRID 460736ノート

反応式

HRID 460736 の反応式
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]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 79372,6-Lutidine2 回HCID 6451240Aluminum(III) ChlorideHCID 178443172N-[4-chloro-3-[[5-oxo-1-(2,4,6-trichlorophenyl)-4H-pyrazol-3-yl]amino]phenyl]tetradecanamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
10 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1e047ed0942046248435f195249898c6
出典データセット
uspto-grants-1977_12
特許番号
US04061498

反応ノート

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