In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 148017-28-1, name is tert-Butyl sulfamoylcarbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: tert-Butyl sulfamoylcarbamate
(S)-(6-chloro-2,3-dihydrobenzo[b][1 ,4]dioxin-2-yl)methanol (20.0 g, 100.0 mmol, 1 .0 eq.), tert-butoxycarbonyl sulfamide (27.4 g, 140.0 mmol, 1 .4 eq) and triphenylphosphine (3.9 g, 1 18.0 mmol, 1 .2 eq,) were dissolved in MTBE (140 g) and the resulting mixture was warmed under stirring to a temperature in the range of 27-32C. Diisopropyl-azodicarboxylate (22.6 g, 1 1 1 .0 mmol, 1 .1 1 eq) in MTBE (18 g) was added dropwise over about 60-120 min, while maintaining the temperature of the reaction mixture in the range of about 27-32C. The resulting mixture was then stirred for 2-6 hours, cooled to a temperature in the range of about 15-20C. The resulting mixture was then seeded with triphenylphosphinoxide and bis-1,2-(isopropoxycarbonyl)-hydrazine (which were taken from previously prepared batches) and stirred for an additional hour. After the onset of crystallization was confirmed, n-hexane (80 g) was added over about 45-60 min, after which time, the resulting suspension was stirred for an additional 120 min at a temperature of about 15-20C. The resulting mixture was then cooled to a temperature in the range of -15 to -10C and stirred for about 4-6 hours. The resulting off-white solid was filtered off and washed with a cold mixture of MTBE (20 g) and n-hexane (10 g). At 50C and a pressure of about 450-400 mbar a total of 240 g of solvent was distilled off from the resulting filtrate. To the resulting concentrated residue were added toluene (100 g) and n-hexane (15 g). The resulting solution, at a temperature of about 22-27C, was washed with a mixture of methanol (40 g) and water (60 g). This step was then repeated twice (2X). At a temperature of about 45C and at about 250-100 mbar pressure, about 90 g of solvent were distilled off to yield a concentrated residue containing the desired product.
The synthetic route of 148017-28-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; JANSSEN PHARMACEUTICA NV; GONG, Yong; ZINSER, Hartmut B.; WO2013/49021; (2013); A1;,
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