تفاعل #64705

ord-336b3b8c2eb143d68f7aa0398be0a69a

معادلة التفاعل

Cl
hydrochloric acid
Cc1ccccc1C(=O)Cl
2-methylbenzoyl chloride
[C-]#[N+]C
methyl isocyanide
O=C([O-])[O-].[Ca+2]
calcium carbonate
CNC(=O)C(=O)c1ccccc1C
title compound
المردود 96.6%
CNC(=O)C(=O)c1ccccc1C
N-methyl-2-(2-tolyl)-2-oxoacetamide
المردود 96.6%

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added
  2. 2
    workup.STIRRINGThe stirring of the resulting mixture
  3. 3
    workup.WAITwas continued for 1 hour
  4. 4
    استخلاصextracted with methylene chloride
  5. 5
    غسيلThe organic layer was washed with saturated brine
  6. 6
    تجفيفdried over anhydrous magnesium sulfate
  7. 7
    أخرىThe solvent was evaporated under reduced pressure
  8. 8
    غسيلeluted with hexane-ethyl acetate (5:1)

الإجراء التجريبي

A mixture of 2-methylbenzoyl chloride (1.55 g) and methyl isocyanide (492 mg) was stirred at 60° C. for 6 hours. Then, the mixture was diluted with acetone (20 ml), and water (4 ml) and calcium carbonate (1.00 g) were added. The stirring of the resulting mixture was continued for 1 hour. The mixture was neutralized with dilute hydrochloric acid and extracted with methylene chloride. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with hexane-ethyl acetate (5:1) to obtain the title compound (1.71 g, Yield: 96.6%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05414122uspto-grants-1995_05