Benzene hexane → 2-Methyl-5-nitrobenzyl acetate

HRID 1388085

반응식

HRID 1388085 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 129407612-Methyl-5-nitrobenzyl acetate

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
115 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-25feafc9070146f49ae4c1ce2acbaf1c
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04430114

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