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Dimethylformamide → HCID 21496591, 화합물

HRID 1730825
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인쇄 미리보기

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HRID 1730825 반응식
[CH2:1]([O:3][CH:4]([C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=1)[CH2:5][CH2:6][CH2:7]Cl)[CH3:2].[CH2:16]([O:18][C:19]1[CH:28]=[CH:27][CH:26]=[CH:25][C:20]=1[O:21][CH2:22][CH2:23][NH2:24])[CH3:17].[C:29](=[O:32])([OH:31])[O-].[Na+].CN(C)C=O>O>[C:4]([OH:3])(=[O:18])[C:29]([OH:31])=[O:32].[CH2:1]([O:3][CH:4]([C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=1)[CH2:5][CH2:6][CH2:7][NH:24][CH2:23][CH2:22][O:21][C:20]1[CH:25]=[CH:26][CH:27]=[CH:28][C:19]=1[O:18][CH2:16][CH3:17])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 516892Sodium BicarbonateHCID 53030422-(2-Ethoxyphenoxy)ethylamineHCID 21496613HCID 21496613, 화합물

생성물 1

HCID 21496591HCID 21496591, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

A mixture of 4.4 g of 4-ethoxy-4-(4-fluorophenyl)-butyl chloride, 3.6 g of 2-(2-ethoxyphenoxy)ethylamine, 2 g of sodium bicarbonate and 44 ml of N,N-dimethylformamide was stirred at about 110° C for 20 hours. After cooling, the reaction mixture was poured into cold water and extracted with benzene. The benzene layer was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The oily residue was treated with ethanolic oxalic acid and recrystallized from ethanol to give N-[4-ethoxy-4-(4-fluorophenyl)butyl]-2-(2-ethoxyphenoxy)-ethylamine oxalate, M.P. 157° - 160° C.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with benzene
  3. washThe benzene layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionThe oily residue was treated with ethanolic oxalic acid
  7. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-b06bd60d568b4661af8b5941a6d78a76
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03993780

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