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N,N-Diethylethylenediamine → HCID 20225376, 화합물

HRID 463679
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HRID 463679 반응식
[CH2:1]([S:3]([NH:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([Cl:13])=[O:12])=[CH:9][CH:8]=1)(=[O:5])=[O:4])[CH3:2].[CH2:16]([N:18]([CH2:22][CH3:23])[CH2:19][CH2:20][NH2:21])[CH3:17]>C1COCC1>[ClH:13].[CH2:16]([N:18]([CH2:22][CH3:23])[CH2:19][CH2:20][NH:21][C:11](=[O:12])[C:10]1[CH:14]=[CH:15][C:7]([NH:6][S:3]([CH2:1][CH3:2])(=[O:5])=[O:4])=[CH:8][CH:9]=1)[CH3:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 60993N,N-DiethylethylenediamineHCID 15057240HCID 15057240, 화합물

생성물 1

HCID 20225376HCID 20225376, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-10 °C

실험 절차

Dissolve 4.97 g (0.22 moles) 4-[(ethylsulfonyl)amino]benzoyl chloride in 25 ml THF. Stir under N2 at -10° C. To the solution add 3.0 ml (0.22 mole) N,N-diethylethylenediamine dropwise. Follow the progress of the reaction by thin layer chromatography on silica gel (acetonitrile:methanol:ammonium hydroxide, 85:10:5). When the reaction is complete, remove the solvents in vacuo. Dissolve the gummy residue in refluxing ethanol and chill to produce white crystals. Filter the precipitate to obtain the title compound.

후처리

  1. customthe progress of the reaction by thin layer chromatography on silica gel (acetonitrile:methanol:ammonium hydroxide, 85:10:5)
  2. customremove the solvents in vacuo
  3. dissolutionDissolve the gummy residue
  4. temperaturein refluxing ethanol
  5. temperaturechill
  6. customto produce white crystals
  7. filtrationFilter the precipitate

출처 및 근거

ORD 기록
ord-58a7057dc0c142358dbba4672ae9632c
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04544654

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