反応 #49959

反応方程式

o-anisidine

benzoyl isothiocyanate

→

N-(o-methoxyphenyl)thiourea

収率 57.1%

溶媒

acetone

反応条件

後処理

1. 1
   温度under reflux for 2 hours
2. 2
   ろ過The resulting crystals were collected by filtration
3. 3
   洗浄washed with cold acetone
4. 4
   その他dried under reduced pressure
5. 5
   workup.ADDITIONThe crystals were added to 50 ml of 30% methylamine-methanol
6. 6
   workup.STIRRINGthe mixture was stirred at room temperature overnight
7. 7
   濃縮The reaction mixture was concentrated to dryness under reduced pressure
8. 8
   洗浄the residue was washed with ethanol-ethyl acetate
9. 9
   その他dried under reduced pressure

実験手順

To 50 ml of acetone were added 2.46 g of o-anisidine and 3.75 g of benzoyl isothiocyanate, and the mixture is stirred under reflux for 2 hours and, then, allowed to stand overnight in a refrigerator at 5° C. The resulting crystals were collected by filtration, washed with cold acetone and dried under reduced pressure. The crystals were added to 50 ml of 30% methylamine-methanol and the mixture was stirred at room temperature overnight. The reaction mixture was concentrated to dryness under reduced pressure, and the residue was washed with ethanol-ethyl acetate and dried under reduced pressure. The procedure provided 2.08 g of N-(o-methoxyphenyl)thiourea.

出典