4-Fluoro-3-methylbenzonitrile → 3-Methyl-4-(methylsulfanyl)benzonitrile

HRID 527372노트

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HRID 527372 반응식
[CH3:1][S-:2].[Na+].F[C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[CH:7][C:6]=1[CH3:13]>CN(C=O)C>[CH3:13][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:5]=1[S:2][CH3:1])[C:9]#[N:10]

참가 물질

4

반응물 2

HCID 27791804-Fluoro-3-methylbenzonitrileHCID 4378561Sodium methanethiolate

생성물 1

HCID 578566063-Methyl-4-(methylsulfanyl)benzonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

Sodium methanethiolate (1.60 g, 22.8 mmol) is added to a solution of 4-fluoro-3-methyl-benzonitrile (2.50 g, 18.5 mmol) in DMF, and the mixture is heated at 80° C. for 15 min. All volatiles are evaporated, and the residue is treated with water. The mixture is extracted with ethyl acetate twice, and the organic layer is dried over Na2SO4 and concentrated. Yield: 3.0 g (99% of theory); ESI mass spectrum: [M+H]+=164; r.t. HPLC: 0.61 min (X011_S03).

후처리

  1. customAll volatiles are evaporated
  2. additionthe residue is treated with water
  3. extractionThe mixture is extracted with ethyl acetate twice
  4. dry with materialthe organic layer is dried over Na2SO4
  5. concentrationconcentrated
  6. customr.t
  7. custom0.61 min (X011_S03)

출처 및 근거

ORD 기록
ord-7407de6ace15485596ad83621c5bd3c0
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346794B1

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