p-Toluenesulfonic acid → HCID 20529068, 화합물

HRID 66763

반응식

HRID 66763 반응식
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

참가 물질

7

반응물 4

HCID 6101p-Toluenesulfonic acid2회HCID 2250301,2-Ethanediamine, 4-methylbenzenesulfonate (1:?)HCID 12832554HCID 12832554, 화합물HCID 13123534HCID 13123534, 화합물

생성물 1

HCID 20529068HCID 20529068, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 72391,2-Dichlorobenzene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-ff23076f9cdd42e0951ae0a9c3896e80
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343810

연결된 노트

불러오는 중…