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

HRID 833

반응식

HRID 833 반응식
[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]

참가 물질

7

반응물 4

HCID 1049PyridineHCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 520718Dinitrobenzonitrile

생성물 1

HCID 151982412-Nitro-6-(phenylthio)benzonitrile수율 89%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-9c0049ffd5bd4c2597bd8dc1da4f9125
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723452

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