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Sodium Iodide → HCID 21496591, 화합물

HRID 1730826
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HRID 1730826 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][NH2:8])[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]Cl)[CH3:17].[I-].[Na+].[C:31](=[O:34])([OH:33])[O-].[Na+]>O.CN(C)C=O>[C:4]([OH:3])(=[O:18])[C:31]([OH:33])=[O:34].[CH2:1]([O:3][CH:4]([C:9]1[CH:10]=[CH:11][C:12]([F:15])=[CH:13][CH:14]=1)[CH2:5][CH2:6][CH2:7][NH:8][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

7

반응물 4

HCID 5238Sodium IodideHCID 516892Sodium BicarbonateHCID 176208991-(2-Chloroethoxy)-2-ethoxybenzeneHCID 21496608HCID 21496608, 화합물

생성물 1

HCID 21496591HCID 21496591, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

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온도
110 °C

실험 절차

A mixture of 2 g of N-[4-ethoxy-4-(4-fluorophenyl)butyl]amine, 2 g of 2-(2-ethoxyphenoxy)ethyl chloride, 0.1 g of sodium iodide, 1 g of sodium bicarbonate and 20 ml of N,N-dimethylformamide was stirred at about 110° C for 20 hours. After cooling, the reaction mixture was poured into 200 ml of water and extracted with benzene. The benzene layer was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The 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 residue was treated with ethanolic oxalic acid
  7. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-5d7e3d0f06e64087ab01e7c6b1776fef
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03993780

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