2-Chloro-6-nitrotoluene → 3-Chloro-2-methylaniline

温度

100 °C

To a mixed solution of 150 g of stannous chloride and 200 ml of concentrated sulfuric acid under ice-cooling is added 29 g of 2-chloro-6-nitrotoluene. Then, the solution is heated at 100° C. for 1 hour, resulting in white crystals. The crystals are recovered by filtration and dissolved in a mixed solution of 400 ml of water and 50 ml of a 40% NaOH solution, followed by extracting with 500 ml of chloroform. After washing the extract with 400 ml of water, the chloroform layer is dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure for concentration. Distillation of the resultant residue yields 23 g of 2-methyl-3-chloroaniline as the fraction of 115°-116° C./10 mmHg.

1. customresulting in white crystals
2. filtrationThe crystals are recovered by filtration
3. dissolutiondissolved in a mixed solution of 400 ml of water and 50 ml of a 40% NaOH solution
4. extractionby extracting with 500 ml of chloroform
5. washAfter washing the
6. extractionextract with 400 ml of water
7. dry with materialthe chloroform layer is dried over anhydrous magnesium sulfate
8. distillationthe solvent is distilled off under reduced pressure for concentration
9. distillationDistillation of the resultant residue

ORDレコード

ord-b54fe42c39d04bc29fcd344182038bb1

出典データセット

uspto-grants-1985_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04544747