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N,N-Diethyl-1,3-propanediamine → HCID 70382571, 화합물

HRID 1608296
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HRID 1608296 반응식
[C:1]1([C:7]2[CH:8]=[N:9][N:10]([CH2:18][CH2:19][C:20]([O:22]C)=[O:21])[C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:24]([N:26]([CH2:29][CH2:30][CH2:31][NH2:32])[CH2:27][CH3:28])[CH3:25]>ClCCl>[OH2:21].[CH2:24]([N:26]([CH2:27][CH3:28])[CH2:29][CH2:30][CH2:31][NH:32][C:20](=[O:22])[CH2:19][CH2:18][N:10]1[C:11]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:8]=[N:9]1)[CH3:25].[CH2:24]([N:26]([CH2:29][CH2:30][CH2:31][NH:32][C:20](=[O:22])[CH2:19][CH2:18][N:10]1[C:11]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:8]=[N:9]1)[CH2:27][CH3:28])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 61011N,N-Diethyl-1,3-propanediamine2회HCID 14723696Methyl 3-(4,5-diphenyl-1H-pyrazol-1-yl)propanoate

생성물 1

HCID 70382571HCID 70382571, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 4.8 g (0.016 mol) of methyl 4,5-diphenyl-1H-pyrazole-1-propanoate of example 4 and 48 mL of diethylaminopropylamine was heated at 120°-125° C. under nitrogen for 14 hours. The excess diethylaminopropylamine was stripped in vacuo at 85° C. The residue was dissolved in dichloromethane, an unwanted solid residue was filtered off, and the methylene chloride solution was washed twice with water and once with brine. The product was extracted into chilled dilute hydrochloric acid, and the chilled aqueous acid was made basic with solid sodium bicarbonate and then sodium carbonate. The basic water was extracted 4 times with dichloromethane, the combined washings were dried over sodium sulfate, and stripped to yield 2.4 g viscous amber oil. The oily product was dried at 40° C. and 0.1 mm vacuum for 7 days to yield 1.6 g of the hemihydrate still as a viscous oil.

후처리

  1. customwas stripped in vacuo at 85° C
  2. filtrationan unwanted solid residue was filtered off
  3. washthe methylene chloride solution was washed twice with water and once with brine
  4. extractionThe product was extracted
  5. temperatureinto chilled dilute hydrochloric acid
  6. extractionThe basic water was extracted 4 times with dichloromethane
  7. dry with materialthe combined washings were dried over sodium sulfate

출처 및 근거

ORD 기록
ord-9fc13b8b33174ef894f08f360501bdc2
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870095

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