3,4-DIMETHYLTHIENO[2,3-B]THIOPHENE synthesis
- Product Name:3,4-DIMETHYLTHIENO[2,3-B]THIOPHENE
- CAS Number:175202-58-1
- Molecular formula:C8H8S2
- Molecular Weight:168.28
Yield:175202-58-1 99.2%
Reaction Conditions:
with 5% rhodium-on-charcoal;potassium tert-butylate at 150; under 6080.41 Torr; for 25 h;Inert atmosphere;Temperature;Pressure;Reagent/catalyst;Concentration;
Steps:
2.1; 2.2 Example 2One-step synthesis of 3,4-dimethylthieno [2,3-b] thiophene, comprising the steps of:
1) Thieno [2,3-b] thiophene, nitromethane, potassium tert-butoxide and5% rhodium carbon mixture, purged with argon, warmed to 150 ,Pressurized to 8 atmospheres, the reaction 25h; wherein thieno [2,3-b] and thiophene,The molar amounts of nitromethane and potassium tert-butoxide were 0.1 mol,4.5 mol and 0.7 mol, the amount of rhodium carbon is 3.2% of the weight of thieno [2,3-b] thiophene;2) After the reaction, the solid rhodium carbon was recovered by filtration, the filtrate was washed with water,Concentration by distillation gave an excess of the substituted methane and 16.68 g of solid 3,4-dimethylthieno [2,3-b] thiophene in 99.2% yield. Recycling of solid rhodium carbon with chloroform after drying can be reused.
References:
CN106986882,2017,A Location in patent:Paragraph 0023; 0024; 0025; 0026; 0027; 0028-0036