Water → HCID 12803422, compound

Temperature

0 °C

Phenacyl bromide (199 g.), in 400 ml. of chloroform, is added over one half hour to a mixture of 2-methoxyethylamine (82 g) and triethylamine (152 g.) in 200 ml. of chloroform at 0° C. The mixture is stirred for two hours at 0°-10° C. Water (400 ml.) is added and the organic layer is separated and washed with another 400 ml. of water. The chloroform layer is cooled to 0° C. with an ice bath and glacial acetic acid (72 g.) potassium cyanate (89 g.) and methanol (100 ml.) are added. The mixture is refluxed for ninety minutes, cooled and washed with saturated sodium bicarbonate solution, and the organic layer is dried over anhydrous sodium sulfate and then concentrated to give a semisolid. Trituration with 300 ml. of ether and filtration gives the title product as a yellow crystal; m.p. 152°-154° C.

1. customat 0° C
2. customthe organic layer is separated
3. washwashed with another 400 ml
4. additionglacial acetic acid (72 g.) potassium cyanate (89 g.) and methanol (100 ml.) are added
5. temperatureThe mixture is refluxed for ninety minutes
6. temperaturecooled
7. washwashed with saturated sodium bicarbonate solution
8. dry with materialthe organic layer is dried over anhydrous sodium sulfate
9. concentrationconcentrated
10. customto give a semisolid
11. filtrationof ether and filtration

ORD record

ord-bb591fc2fd4548659e59c050add1e6da

Source dataset

uspto-grants-1986_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04620009