HRID364916
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
38.6 g of 3-amino-9-ethylcarbazole and 27.9 ml of triethylamine were added to 300 ml of methanol, and, while cooling with ice, 15.2 g of carbon disulfide was added dropwise thereto. After conducting reaction at room temperature for 3 hours, 41.3 g of dicyclohexylcarbodiimide was added thereto, followed by reacting at room temperature for 4 hours. Crystals thus precipitated were collected by filtration, heat-refluxed for 10 minutes in 500 ml of ethyl acetate, and cooled to precipitate and then filter off solids. The filtrate was concentrated by removing solvents in vacuo to obtain the desired product (29 g).
WORKUP
后处理
- additionwas added dropwise
- customreaction at room temperature for 3 hours
- customCrystals thus precipitated
- filtrationwere collected by filtration
- temperatureheat-refluxed for 10 minutes in 500 ml of ethyl acetate
- temperaturecooled
- customto precipitate
- filtrationfilter off solids
- concentrationThe filtrate was concentrated
- customby removing solvents in vacuo