Ammonia → N-(2-phenoxypropyl)phenylacetamidine p-toluenesulphonate

HRID 1288227

反応式

HRID 1288227 の反応式
[O:1]([CH:8]([CH3:11])[CH2:9][NH2:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:12]1([CH3:22])[CH:17]=[CH:16][C:15]([S:18]([OH:21])(=[O:20])=[O:19])=[CH:14][CH:13]=1.[C:23]1([CH2:29][C:30](N)=[NH:31])[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.N>C(O)C.CCOCC>[C:12]1([CH3:22])[CH:13]=[CH:14][C:15]([S:18]([OH:21])(=[O:19])=[O:20])=[CH:16][CH:17]=1.[O:1]([CH:8]([CH3:11])[CH2:9][NH:10][C:30](=[NH:31])[CH2:29][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 222AmmoniaHCID 37183552-Phenoxy-1-propanamineHCID 21504266Phenylacetamidine p-toluenesulphonate

生成物 1

HCID 178457535N-(2-phenoxypropyl)phenylacetamidine p-toluenesulphonate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

2-Phenoxypropylamine (6.0 g.) was added to a suspension of phenylacetamidine p-toluenesulphonate (12.4 g.) in absolute ethanol (20 ml.). The mixture was heated to reflux for 4 hours by which time the initially vigorous evolution of ammonia had practically ceased. The resulting solution was cooled somewhat and diluted with ether to give an oil which rapidly crystallised on scratching. The solid was filtered and recrystallised from a mixture of ethanol and water to give N-(2-phenoxypropyl)phenylacetamidine p-toluenesulphonate, m.p. 127°-129°.

後処理

  1. temperatureThe mixture was heated
  2. temperatureThe resulting solution was cooled somewhat
  3. customto give an oil which
  4. customrapidly crystallised
  5. filtrationThe solid was filtered
  6. customrecrystallised from a mixture of ethanol and water

出典と根拠

ORDレコード
ord-719982c498de4dda8dc06af693ee3417
出典データセット
uspto-grants-1976_10
特許番号
US03987158

関連ノート

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