Pyridine → 2-Nitro-6-(phenylthio)benzonitrile

HRID 833

反応式

HRID 833 の反応式
[N+]([C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[C:5]=1[C:6]#[N:7])([O-])=O.[C:15]1([SH:21])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C([O-])([O-])=O.[K+].[K+].N1C=CC=CC=1>CN(C=O)C.O>[N+:12]([C:8]1[CH:9]=[CH:10][CH:11]=[C:4]([S:21][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:5]=1[C:6]#[N:7])([O-:14])=[O:13]

参加物

7

反応物 4

HCID 1049PyridineHCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 520718Dinitrobenzonitrile

生成物 1

HCID 151982412-Nitro-6-(phenylthio)benzonitrile収率 89%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

An ice water bath-cooled mixture of 2.0 g (0.01 mol) of 2,6-dinitrobenzonitrile (Lancaster Synthesis, Inc., Windham, N.H. 03087), 1.06 ml (0.01 mol) of thiophenol, and 1.44 g (0.01 mol) of anhydrous K2CO3 in 50 mL of DMF was stirred for 0.5 h. Pyridine was added to the reaction mixture until it became basic, and was followed by the addition of approximately 100 mL of H2O. The yellow precipitate was collected by filtration, washed with 1N NaOH, water and dried to give 1.94 g (89%) of 2-nitro-6-(phenylthio)benzonitrile as a yellow solid: mp 106°-107° C.

後処理

  1. filtrationThe yellow precipitate was collected by filtration
  2. washwashed with 1N NaOH, water
  3. customdried

出典と根拠

ORDレコード
ord-9c0049ffd5bd4c2597bd8dc1da4f9125
出典データセット
uspto-grants-1998_03
特許番号
US05723452

関連ノート

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