反応 #41507

反応方程式

water

4-bromoguaiacol

1,4-diazabicyclo(2.2.2)octane

NMP

dimethylthiocarbamoyl chloride

NMP

→

O-4-bromo-2-methoxyphenyl dimethylcarbamothioate

反応条件

後処理

1. 1
   その他to give a dark-yellow solution
2. 2
   その他Some precipitated has formed during the addition
3. 3
   workup.STIRRINGThe mixture was stirred overnight at r.t.
4. 4
   その他the precipitate was isolated by filtration
5. 5
   洗浄washed twice with water
6. 6
   その他dried in vacuo at 50° C.
7. 7
   その他to yield a pale creamed-coloured crystalline solid, 2.11 g (72%)

実験手順

A mixture of 4-bromoguaiacol (2.05 g, 10.1 mmol) and 1,4-diazabicyclo(2.2.2)octane (1.42 g, 12.6 mmol) in NMP (24 mL) was heated at 50° C. to give a dark-yellow solution. A solution of dimethylthiocarbamoyl chloride (1.37 g, 11.1 mmol) in NMP (2 ml) was added dropwise to the previous solution over 1-2 min. Some precipitated has formed during the addition. The mixture was stirred at 50° C. for 3 h, and then water (25 ml) was added over 5 min at 50° C. The mixture was stirred overnight at r.t., and the precipitate was isolated by filtration, washed twice with water, and dried in vacuo at 50° C. to yield a pale creamed-coloured crystalline solid, 2.11 g (72%).

出典