Benzene hexane → 2-Methyl-5-nitrobenzyl acetate

HRID 1388085

反応式

HRID 1388085 の反応式
[C:1]([O-:4])(=[O:3])[CH3:2].[Na+].[CH3:6][C:7]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:8]=1[CH2:9]Cl.CCCCCC.C1C=CC=CC=1>C(O)(=O)C>[C:1]([O:4][CH2:9][C:8]1[CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=[CH:14][C:7]=1[CH3:6])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 110624Benzene hexaneHCID 1879522-(Chloromethyl)-1-methyl-4-nitrobenzeneHCID 517045Sodium Acetate

生成物 1

HCID 129407612-Methyl-5-nitrobenzyl acetate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
115 °C

実験手順

A slurry of anhydrous sodium acetate (60.0 g; 0.73 mol) in acetic acid (400 ml) is stirred and 2-methyl-5-nitrobenzyl chloride (45.3 g; 0.24 mol) added. The resulting reaction mixture is heated to reflux and is heated overnight at 115° C., after which time tlc (silica gel; 75/25 hexane/benzene) indicates that no starting material is present. The mixture is cooled down, concentrated in vacuo, and diluted with water. The precipitated solid (48.9 g; 95.8%) is collected and dried. A sample recrystallized from hexane has a melting point of 52°-53.5° C.

後処理

  1. customThe resulting reaction mixture
  2. temperatureis heated
  3. temperatureto reflux
  4. temperatureThe mixture is cooled down
  5. concentrationconcentrated in vacuo
  6. additiondiluted with water
  7. customThe precipitated solid (48.9 g; 95.8%) is collected
  8. customdried
  9. customA sample recrystallized from hexane

出典と根拠

ORDレコード
ord-25feafc9070146f49ae4c1ce2acbaf1c
出典データセット
uspto-grants-1984_02
特許番号
US04430114

関連ノート

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