Water → O-4-bromo-2-methoxyphenyl dimethylcarbamothioate

Temperatur

50 °C

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%).

1. customto give a dark-yellow solution
2. customSome precipitated has formed during the addition
3. stirringThe mixture was stirred overnight at r.t.
4. customthe precipitate was isolated by filtration
5. washwashed twice with water
6. customdried in vacuo at 50° C.
7. customto yield a pale creamed-coloured crystalline solid, 2.11 g (72%)

ORD-Eintrag

ord-22927637731c442b9632d5b40b43532b

Quelldatensatz

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07728030B2