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Benzyltrimethylammonium hydroxide → HCID 70546733, 화합물

HRID 2057375
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HRID 2057375 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N:9]([C:13]1[NH:14][CH2:15][CH2:16][N:17]=1)[CH2:10][C:11]#[CH:12].[OH-].C[N+](C)(C)CC1C=CC=CC=1>C(O)C>[Cl:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[N:9]1[C:13]2=[N:14][CH2:15][CH2:16][N:17]2[C:11]([CH3:12])=[CH:10]1
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참가 물질

4

반응물 2

HCID 66854Benzyltrimethylammonium hydroxideHCID 20332207N-(2,6-Dichlorophenyl)-N-(prop-2-yn-1-yl)-4,5-dihydro-1H-imidazol-2-amine

생성물 1

HCID 70546733HCID 70546733, 화합물수율 18.7%

시약·촉매·용매 1

HCID 702Ethanol촉매

실험 절차

A mixture consisting of 5.4 gm of 2-[N-(2,6-dichloro-phenyl)-N-propargyl-amino]-2-imidazoline and 40 ml of ethanol containing 5 drops of trimethylbenzyl ammonium hydroxide was refluxed for five hours, while stirring. Thereafter, the ethanol was evaporated in vacuo, and the residue was dissolved in dilute hydrochloric acid. The resulting solution was fractionally extracted with ether at stepwisely increasing pH-values (addition of 2 N sodium hydroxide). The thin-layer chromatographically uniform ethereal fractions having a pH of 9 or more were combined, dried over magnesium sulfate, and the ether was evaporated in vacuo, leaving 1 gm (18.7% of theory) of 7-(2,6-dichloro-phenyl)-2,3-dihydro-5-methyl-imidazo[1,2-α]imidazole, m.p. 113°-117° C.

후처리

  1. temperaturewas refluxed for five hours
  2. customThereafter, the ethanol was evaporated in vacuo
  3. dissolutionthe residue was dissolved in dilute hydrochloric acid
  4. extractionThe resulting solution was fractionally extracted with ether at stepwisely increasing pH-values (addition of 2 N sodium hydroxide)
  5. dry with materialdried over magnesium sulfate
  6. customthe ether was evaporated in vacuo

출처 및 근거

ORD 기록
ord-03058b514d05496faa348475546a3566
출처 데이터셋
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04210659

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