1,3-Dianilinopropane → HCID 12069779、化合物

HRID 379204ノート

反応式

HRID 379204 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[CH:13]=[CH:14]/[CH:15]=[CH:16]/[C:17](Cl)=[O:18])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[C:20]1([NH:26][CH2:27][CH2:28][CH2:29][NH:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.[C:37](=[O:40])([O-])O.[Na+]>C(Cl)Cl.N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[CH:13]=[CH:14]/[CH:15]=[CH:16]/[C:17]([N:30]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH2:29][CH2:28][CH2:27][N:26]([C:37](=[O:40])/[CH:16]=[CH:15]/[CH:14]=[CH:13]/[C:5]2[CH:6]=[C:7]([O:11][CH3:12])[C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[O:18])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10]

参加物

6

反応物 3

HCID 669161,3-DianilinopropaneHCID 516892Sodium BicarbonateHCID 22609552HCID 22609552、化合物

生成物 1

HCID 12069779HCID 12069779、化合物収率 59%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 5-(3,4,5-trimethoxyphenyl)penta-(2E,4E)-dienoyl chloride in methylene chloride (3 ml) was added dropwise to a solution of 68 mg (0.30 mmol) of N,N′-diphenyl-1,3-diaminopropane in pyridine (3 ml) with stirring in an ice bath. After completion of the addition, the mixture was stirred for an additional 1 hour, and a 5% aqueous solution (5 ml) of sodium hydrogencarbonate was added to the reaction mixture to conduct extraction with chloroform. An organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resultant crude oil (278 mg) was purified by column chromatography on silica gel, thereby obtaining 126 mg (yield: 59%) of the title compound as a colorless amorphous powder.

後処理

  1. additionAfter completion of the addition
  2. stirringthe mixture was stirred for an additional 1 hour
  3. extractionextraction with chloroform
  4. dry with materialAn organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resultant crude oil (278 mg) was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-e44b15da458b4e0d9b374bc6bc938466
出典データセット
uspto-grants-2001_10
特許番号
US06297283B1

反応ノート

読み込み中…