Patent GB607765 (http://l2.espacenet.com/dips/viewer?PN=GB607765&CY=gb&LG=en&DB=EPD)
Carboxylic amides are prepared by heating acyclically unsaturated compounds with sulphur and basic trivalent nitrogen compounds which have hydrogen attached to the nitrogen. The unsaturated compound may contain an olefinic or acetylenic linkage and may be a hydrocarbon or may also contain groups such as the ether, ester, ketone, aldehyde, amide, carboxylic acid or alcohol group, and examples are given of many such compounds and also of suitable nitrogen compounds. The reaction may be carried out in an aqueous or organic solvent. The sulphur may be used in the reaction mixture as flowers of sulphur or may be dissolved in the nitrogen base as a polysulphide. Examples are given of the production of (1) phenylacetamide from styrene, aqueous ammonia and sulphur in pyridine; (2) phenylacetamide from phenylacetylene, sulphur and aqueous ammonia in pyridine; (3) phenylacetamide from phenylacetylene and ammonium sulphide-sulphur in dioxane; (4) phenylacetamide from styrene and ammonium sulphide-sulphur in dioxane; (5) phenylacetothiomorpholide from styrene, sulphur and morpholine; (6) phenylacetothiomorpholide from phenylacetylene, sulphur and morpholine; (7) b -phenylpropionamide from 1-phenylpropene-1, sulphur and ammonium sulphide solution in pyridine; (8) b -phenylpropionamide from 1-phenylpropene-1, sulphur and aqueous ammonia in pyridine; (9) b -phenylpropionamide from 1-methyl-2-phenylacetylene, ammonium sulphide solution and sulphur in pyridine; (10) n-heptamide from 1-heptene, ammonium sulphide solution and sulphur in pyridine; (11) n-heptamide from 1-heptene, aqueous ammonia and sulphur in pyridine; (12) a -phenylpropionamide from a -methylstyrene, aqueous ammonia and sulphur in pyridine; (13) 2-naphthylacetothiomorpholide from 2-naphthylethylene, sulphur and morpholine and b -(2,4 - dichlorophenoxy) - propiothiomorpholide from 2,4-dichlorophenylallyl ether, sulphur and morpholine-the former may be converted to the corresponding carboxylic acid by hydrolysis in presence of acetic and hydrochloric acids-and (14) 2-pyridylacetamide from 2-vinylpyridine, sulphur and aqueous ammonia in pyridine.
The procedure described by tweekdexter was published in The-Hive
Post 258134 (missing)
(foxy2: "New preparation of phenylacetic acid", Chemistry Discourse)
and the Chinese patent Patent CN1110677 (http://l2.espacenet.com/dips/viewer?PN=CN1110677&CY=gb&LG=en&DB=EPD)
uses:
21,7 g
37,6 g
50 ml
30 ml
But my Chinese is too bad, to seee what chemical is 21,7 g etc.
:)
Phenylacetamide to Phenylacetic acid:
Organic Syntheses CV 4, 760
http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=CV4P0760 (http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=CV4P0760)
They use aqueous ammonia ? percentage ? and ethanol in 95% ?
They don't say. I guess that's part of the proprietary secret. The ammonia is aqueous, percentage unknown, and I would imagine that a little water in the alcohol wouldn't matter, seeing as how the ammonia is dissolved in water. :)
Perhaps from stoichiometry it could bee guestimated. I would imagine it would be one of the standard percentages, like 10 or 28 %. My money's on 7 or 10%.
More of the patent:
Preparation of styrene:
A distillation setup was assembled. 100 g powdered scrap polystyrene was added and heated to 340 C or higher. Distillate over 340 C was collected and assumed to be styrene. Still, color was rather crimson, and impure. The impure product was mixed uniformly with 5% by volume sulfuric acid and let stand for 3h to remove impurities, then rinsed 3 times with brine, dried with anhydrous sodium sulfate, added antipolymerization additives. The portion boiling at 145-146 C was collected to yield 89 g (89%) styrene.