Sodium Chloride → 4-(5,6,7,8-Tetrahydroquinoline-8-ylthio)-benzonitrile

HRID 231541

반응식

HRID 231541 반응식
Cl.Cl[CH:3]1[C:12]2[N:11]=[CH:10][CH:9]=[CH:8][C:7]=2[CH2:6][CH2:5][CH2:4]1.[SH:13][C:14]1[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+].[Cl-].[Na+]>CN(C)C=O>[N:11]1[C:12]2[CH:3]([S:13][C:14]3[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[CH:16][CH:15]=3)[CH2:4][CH2:5][CH2:6][C:7]=2[CH:8]=[CH:9][CH:10]=1

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 11430Potassium CarbonateHCID 5850584-ThiobenzonitrileHCID 137121818-Chloro-5,6,7,8-tetrahydroquinoline hydrochloride

생성물 1

HCID 142812494-(5,6,7,8-Tetrahydroquinoline-8-ylthio)-benzonitrile수율 89%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4.08 g (20 mmol) of 8-chloro-5,6,7,8-tetrahydroquinoline hydrochloride, 3.38 g (25 mmol) of 4-mercaptobenzonitrile and 6.91 g (50 mmol) of potassium carbonate in 34 ml of dimethylformamide was stirred under nitrogen at room temperature overnight. The mixture was poured into aqueous saturated sodium chloride and was extracted with ethyl acetate. The extract was washed with ice-cold aqueous 2N sodium hydroxide and water, dried over MgSO4 and evaporated under reduced pressure to obtain 4.72 g (89%) of 4-(5,6,7,8-tetrahydroquinoline-8-ylthio)-benzonitrile as colorless crystals (from methanoldichloromethane).

후처리

  1. extractionwas extracted with ethyl acetate
  2. washThe extract was washed with ice-cold aqueous 2N sodium hydroxide and water
  3. dry with materialdried over MgSO4
  4. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b9bf01850e74443aa7151a3d49129b30
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04847268

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