CAS号 [59-67-6] 生产工艺  吡啶-3-甲酸（烟酸）

CAS名: 3-Pyridinecarboxylic acid. 参考文献: Beil. 22, 38; E¹, 503; E², 32; E^3/4, 348.

用途: 医药。C.I.活性黄178。 C.I.活性红221。C.I.活性蓝 187, 216。

生产工艺文献:

BIOS Trip No. 1155. 197. Nicotinic Acid.  英国人译自德文。未说明资料来源。抄录如下。

反应式: 本人有加注。暂未找到相应的德文原件。
 

Quinolinic acid:

    A large iron vessel, Provided with stirrer and jacket for brine cooling and heating, is charged with a mixture of water (3,000 ltr.), quinoline (13 kg.) and calcium carbonate (26 kg.). The mixture is stirred and a temperature of 20⁰C maintained during the addition of potassium permanganate (106 kg.) over a period of 6 hours. When the addition of permanganate is complete the reaction mixture is warmed to a temperature of 90⁰C and the manganese dioxide filtered through a press filter. This filtrate is evaporated in vacuo to a volume of 200 ltr. And the quinolinic acid precipitated from this concentrate by the addition of hydrochloric acid in a lead-line vessel. The product is filtered on a rubber-lined centrifuge and dried.    Yield: 52-53%.

Nicotinic acid:

The reaction vessel is a steel autoclave which is provided with V4A or stoneware liner and has direct gas heating. The vessel is charged with a mixture of qyinolinic acid (15 kg.) and water (150 kg.) and the mixture heated to a temperature of 140⁰C (pressure 23 ats.), this temperature being maintained for 3 hours. The reaction liquid is released under pressure into a V2A steel vessel, where the product crystallizes on cooling. The nicotinic acid is filtered on a vacuum stoneware filter, washed with water and dried.

Yield: 100%.

上海医药产品生产工艺汇编。1966年。P. 269-270. 烟酸 Acidum Nicotinicum (Niacin)（一）淮海制药厂。    抄录如下。

    1. 氧化，脱羧:  配料比  喹啉：硫酸：硝酸：盐酸 = 1: 4.90: 3.9: 0.057

将硫酸，喹啉依次加入搪瓷反应罐内，搅拌加热至150-160⁰ 保温5小时，升温至180⁰， 缓缓滴加硝酸与盐酸的混酸，温度控制在180-220⁰，约需36-40小时加完，在200-230⁰搅拌保温2-3小时，得粗烟酸溶液。

2. 精制:  配料比  喹啉：硫酸铜 = 1: 0.74

将粗制烟酸溶液加1倍量的水稀释，滴加30-33%的液碱至pH 8-9,放冷，甩除硫酸钠与硝酸钠结晶，滤液在搅拌，加热情况下缓缓加入硫酸铜溶液，至烟酸成为铜盐完全沉淀析出，放冷，甩滤得烟酸铜盐，水洗，甩干，将铜盐于适量水相混，通蒸气加热，滴加液碱至pH 9以上，液体不再显绿色，放冷，过滤除去氧化铜。在滤液中，加硫化钠溶液至不再发生黑色沉淀，过滤。滤液浓缩，放冷，加盐酸至pH 3.5-3.9，放冷，甩滤得烟酸粗品。在粗品中加约12倍蒸馏水，活性炭，煮沸，抽滤，放冷，烟酸析出，过滤得成品烟酸。

总收率  39.63% （对喹啉计）。

（二）河北制药厂。  以混合甲基吡啶为原料，略！ 

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发现一些手册，列有上述产品国内生产工艺，但未注明资料来源？

陈忠源  2017年3月1日            于 无锡   明辉国际。