반응 #1174563

반응 방정식

Water

product

2-(1-Hydroxaminoethyl)phenoxathiin

trimethylsilyl isocyanate

→

title compound

N-[1-(Phenoxathiin-2-yl)ethyl]-N-hydroxy urea

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITwas continued for 10 minutes
3. 3
   기타the THF was evaporated
4. 4
   추출the residue was extracted twice with ether
5. 5
   기타the crude product obtained from evaporation of the extracts
6. 6
   기타was crystallized from ether

실험 절차

To a solution of the product from Step 2 (250 mg, 0.965 mmol) in tetrahydrofuran (THF, 4 mL) there was added 85% trimethylsilyl isocyanate (196 mg, 1.45 mmol) and the solution was stirred at room temperature for 1 hour. Water (4 mL) was added, stirring was continued for 10 minutes, then the THF was evaporated; the residue was extracted twice with ether and the crude product obtained from evaporation of the extracts was crystallized from ether to afford the title compound as white crystals, m.p.: dec 155° C. with gassing.

출처