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

HRID 231541

反応式

HRID 231541 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b9bf01850e74443aa7151a3d49129b30
出典データセット
uspto-grants-1989_07
特許番号
US04847268

関連ノート

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