Hydrochloric Acid → 3-Methyl-4-nitrobenzonitrile

HRID 1087123

反応式

HRID 1087123 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 28014343-Methyl-4-nitrobenzonitrile収率 93.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b830a3aaa8c5415f9c4da848718c690f
出典データセット
uspto-grants-1991_07
特許番号
US05034410

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