p-Toluenesulfonic acid → HCID 20529068、化合物

HRID 66763

反応式

HRID 66763 の反応式
ClC1C=CC=CC=1NCC#N.[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(N)CN.CC1C=CC(S(O)(=O)=O)=CC=1.[Cl:38][C:39]1[CH:51]=[CH:50][CH:49]=[CH:48][C:40]=1[NH:41][CH2:42][C:43]1[NH:44][CH2:45][CH2:46][N:47]=1>O.ClC1C=CC=CC=1Cl>[C:12]1([CH3:22])[CH:13]=[CH:14][C:15]([S:18]([OH:21])(=[O:19])=[O:20])=[CH:16][CH:17]=1.[Cl:38][C:39]1[CH:51]=[CH:50][CH:49]=[CH:48][C:40]=1[NH:41][CH2:42][C:43]1[NH:47][CH2:46][CH2:45][N:44]=1

参加物

7

反応物 4

HCID 6101p-Toluenesulfonic acid2 回HCID 2250301,2-Ethanediamine, 4-methylbenzenesulfonate (1:?)HCID 12832554HCID 12832554、化合物HCID 13123534HCID 13123534、化合物

生成物 1

HCID 20529068HCID 20529068、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 72391,2-Dichlorobenzene溶媒

実験手順

The compound 2-((2-chloroanilino)methyl)-2-imidazoline p-toluenesulfonate was prepared using substantially the same procedure described above by heating a mixture of o-chloroanilinoacetonitrile (43.9 g), ethylenediamine p-toluenesulfonate (61.5 g) and 1,2-dichlorobenzene (198 ml). The p-toluenesulfonate salt was hydrolyzed to the free base, i.e., 2-((2-chloroanilino)methyl)-2-imidazoline by slurrying the p-toluenesulfonate salt in water, basifying the slurry and extracting the mixture with CH2Cl2. The methylene chloride was evaporated leaving 38.0 g of the free base. The free base was put in solution in isopropyl alcohol and acidified with hydrochloric acid in isopropyl alcohol which resulted in crystal formation.

後処理

  1. temperatureby heating
  2. extractionextracting the mixture with CH2Cl2
  3. customThe methylene chloride was evaporated

出典と根拠

ORDレコード
ord-ff23076f9cdd42e0951ae0a9c3896e80
出典データセット
uspto-grants-1982_08
特許番号
US04343810

関連ノート

読み込み中…