Reference of 41253-21-8, A common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, molecular formula is C2H2N3Na, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A suspension of 18 g sodium triazolide in 170 g DMF was heated to 90C. At this temperature 47,3 g of 78,3 wt-% racemic (3SR,7RS)-7-(4-chloro-benzyl)-4,4-dimethyl-1 – oxa-spiro[2.4]heptane (racemic mixture of IXa/IXb), prepared according to example 10, were added, followed by stirring of the mixture for 6 h at 90C. Then 129 g of the DMF were distilled off at 50C/3mbar. To the resulting residue 87 g water and 320 g of MCH were added and the phases were separated at 65C. The aqueous phase was extracted with 100 g fresh MCH at 65C. The combined MCH solutions were washed three times with 80 g water. Thereafter the MCH solution was concentrated to 309 g at 80C/500-400 mbar. For crystallization the solution was cooled from 80C to 0C with a rate of 6K/h. After stirring overnight the product was isolated by filtration. The filter cake was washed twice with 50 g of ice-cold MCH and then dried in a vacuum dryer at 50C/8 mbar. Thus 36.4 g of cis-metconazole were obtained, having a purity of 97.1 %, determined by quantitative GC-analysis, corresponding to a yield of 74.5%. Melting point: 1 12C H-NMR (500 MHz, CDCI3): delta/ppm = 0.62 (s, 3H), 1 .04 (s, 3H), 1 .28-1 .48 (m, 2H), 1 .64-1 .82 (m, 2H), 2.25 -2.52, (m, 3H), 3.87-3.94 (s, broad OH), 4.19 (d, 1 H) 4.28 (d, 1 H), 7.10 (d, 2H), 7.20 (d, 2 H), 7,.98 (s, 1 H), 8.21 (s, 1 H) 3C-NMR (125 MHz, CDC ): delta /ppm = 21 .94 (q), 25.08 (q), 27.20 (t), 35.83 (t), 38.07 (t), 46.29 (s), 46.86 (d), 53.92 (t), 82.37 (s), 128.36 (d, 2C), 130.19 (d, 2C), 131.46 (s), 139.71 (s), 144.30 (d), 151.37 (d)
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; BASF AGRO B.V., ARNHEM (NL), ZUeRICH-BRANCH; ZIERKE, Thomas; KEMPER, Paul; WO2013/117629; (2013); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics