| 摘要 |
<p>Sulphuric acid diamides of formula R-C6H4-NH-SO2-NME (I) (where R is H, Me, F or Cl) are prepd. by reacting dimethylamino-sulphochloride having formula Cl-SO2-NMe2 (II) with an aniline having formula R-C6H4-NH2 (III), in the presence of inorganic reducing agents, (IV), and of acid binders, at pH 3-5, 40-80 (45-70) degrees C, in water as diluent. (I) are intermediates in synthesis of pesticides, plant-protective fungicides and dyes. (i) Addn. of (IV) gives a smooth, quicker reaction. (ii) Highly pure (I) is obtd., requiring no further purificn., the moisture content being low. (ii) Cooling may take place by using warm industrial recycle water. In an example, use of NaHSO3 as (IV), in prepn. of PhNH-SO2-NME2 from (II) and aniline, increases yield from 82- to 92%; reduces reaction time from 30- to 20 hrs., increases purity to 99% and reduces moisture content from 25- to 8%.</p> |
