1,3-Dianilinopropane → HCID 12069779, 화합물

HRID 1368925노트

반응식

HRID 1368925 반응식
[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]

참가 물질

6

반응물 3

HCID 669161,3-DianilinopropaneHCID 516892Sodium BicarbonateHCID 22609552HCID 22609552, 화합물

생성물 1

HCID 12069779HCID 12069779, 화합물수율 59%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-19f8236f162342939b3608053cedfcda
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06576642B2

반응 노트

불러오는 중…