CAS号 [79-72-1] 生产工艺。  2-甲基-5-氨基苯磺酰苯胺

CAS名：Benzenesulfonamide, 3-amino-6-methyl-N-phenyl-   历史参考文献：待检索。

用途：酸性黄25, 48。酸性橙19, 41。有机合成等。LookChem网登录生产与经营单位41家。 反应类别：硝基还原。

BIOS 1153, 120. （=胶卷PB85687）。 p-Toluidine-2-sulphonanilide. (Leverkusen).  英国人译自德文（无资料来源）。

反应式：本人有加注，暂未找到德文原件。

3500 l. of wash liquor (from a previous batch), 600 kg. of iron powder and 60-80 l. of hydrochloric acid are charged to the reducer and heated to 800.  The anilide is then slowly charged in, with the temperature rising to 950.  It is finally reduced at the boil untile a sample heated with caustic liquor, filtered, acidified and diluted gives only a trace of turbidity. 

The soluble iron is then precipitated with 12 l. of milk of lime.  After cooling to 700, 30% caustic liquor is added (700 kg.) and the batch tested.

Test: 1/2 l. of the sludge is slurried with hot water, heated to 800, filtered, well washed and extracted with hot 15% caustic liquor.  The estimation of the extract gives the value of the caustic soluble products.  If this is less than 0.15 g. NaNO2, it is filtered.

The liquor is at 50-600 and is acidified with 400 kg. of 600Be’ H2SO4 and then neutralized with soda.  First of all sufficient liquor is run to the acidification vat to allow agitation and then both acid and liquor are run in simultaneously.

For a first batch a little of the product is charged in to help the physical form.  Once the product has started to separate no more lumps are formed.  The press is washed with water until the vat is nearly full.  A further 3500 l. go back to the reduction vessel for the next batch.  After addition of sodium acetate to neutralize (no more precipitate), the product is filtered and well washed with water.   Yield: 94-95%.

张澍声 《精细化工中间体工业生产技术》 1996年。 P. 66.  3-磺酰苯胺基对甲苯胺。 译自BIOS 1153, 120.

还原：将3500 L上一批的洗水，600 kg 铁粉和60-80 L盐酸加到12000 L还原器中，加热至80℃，然后缓缓加入上述磺酰苯胺，温度升至95℃，最后在沸腾下还原。取样与氢氧化钠溶液加热，过滤，酸化，稀释，仅有微量浑浊，即为还原完成。可溶性铁用12 L石灰乳使其沉淀，冷却到70℃，加入700 kg 30% 氢氧化钠溶液。

检验：取0.5 L铁泥，用热水打浆，加热至80℃，过滤，很好洗涤，用15% 热氢氧化钠溶液萃取。萃取物的的测定给出苛性钠可溶产品的值。如该结果少于0.15 g NaNO2 ,即可过滤。

反应混合物现为50-60℃，用400 kg 600波美硫酸酸化，然后用碳酸钠中和，首先将足够量的反应混合物流入反应槽中。将其搅拌，然后将反应混合物和酸同时流入。对于第一锅，应先加入少量产品，有助于产品的物理形态。一经开始分出产品，即不再有大块形成。

压滤，压滤物水洗，3500 L洗水回到还原器中，用于下一批次还原，加入醋酸钠中和后（不用再沉淀），产品过滤，用水很好洗涤。产品得率 94-95%。

抄注：本产品国内未见有报导。

陈忠源 2018年9月26日。