Diisopropylethylamine → 4-Methyl-phenyl sulfamic acid-[6-chloro-5-(p-tolyl)-4-pyrimidinyl]-amide

To 4,6-dichloro-5-p-tolyl-pyrimidine (Referential Example 7) (2.0 g) dissolved in DMSO (35 ml) was added di-isopropyl-ethyl-amine (1.46 ml) followed by addition of 4-methyl-phenyl sulfamic acid amide potassium salt (2.78 g) [prepared from the product described in Referential Example 19 and potassium tert.-butylate in methanol followed by evaporation of the solvent]. The mixture was stirred for 48 h at rt then poured onto water (500 ml) and diethylether (250 ml) was added and the solution was stirred for 30 min. The layers were separated and the water layer was acidified with acetic acid (2.0 ml) and cooled to 0° C. for 1 h. The precipitated product was filtered off and washed with water and diethylether and dried to give 4-methyl-phenyl sulfamic acid-[6-chloro-5-(p-tolyl)-4-pyrimidinyl]-amide (2.02 g). tR=5.00 min (LC); [M+H]+=389.11 (ES+);

1. customprepared from the product
2. customfollowed by evaporation of the solvent]
3. additionthen poured onto water (500 ml) and diethylether (250 ml)
4. additionwas added
5. stirringthe solution was stirred for 30 min
6. customThe layers were separated
7. temperaturecooled to 0° C. for 1 h
8. filtrationThe precipitated product was filtered off
9. washwashed with water and diethylether
10. customdried

ORD-Eintrag

ord-74338b5aed30449facdcc0ace8215f09

Quelldatensatz

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07094781B2