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Benzyltrimethylammonium hydroxide → HCID 70546733、化合物

HRID 2057375
ノート
印刷プレビュー

反応式

HRID 2057375 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 70546733HCID 70546733、化合物収率 18.7%

試薬・触媒・溶媒 1

HCID 702Ethanol触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-03058b514d05496faa348475546a3566
出典データセット
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04210659

反応ノート

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