Hydrochloric Acid → 3-Methyl-4-nitrobenzonitrile

HRID 1087123

반응식

HRID 1087123 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:5]([NH2:7])=O.N1C=CC=CC=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.Cl>ClCCl>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:5]#[N:7]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 9845Trifluoroacetic anhydrideHCID 5959003-Methyl-4-nitrobenzamide

생성물 1

HCID 28014343-Methyl-4-nitrobenzonitrile수율 93.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

To a stirred, 0° C. solution of 3-methyl-4-nitrobenzamide (30 g, 0.169 mol) in dichloromethane (900 mL) under nitrogen was added pyridine (29.5 g, 0.373 mol), then dropwise trifluoroacetic anhydride (42.7 g, 0.203 mol) in dichloromethane (90 mL). The reaction mixture was stirred at 0° C. for one hour and then 1N HCl was added. The organic phase was separated, dried (Na2SO4) and concentrated under reduced pressure to afford 25.5 g (93%) of the 3-methyl-4-nitrobenzonitrile as a light yellow solid; m.p. 69°-71° C.

후처리

  1. customThe organic phase was separated
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b830a3aaa8c5415f9c4da848718c690f
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034410

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