تفاعل #10342

معادلة التفاعل

di-isopropyl-ethyl-amine

4,6-dichloro-5-p-tolyl-pyrimidine

4,6-dichloro-5-(p-tolyl)-pyrimidine

4-methyl-phenyl sulfamic acid amide potassium salt

→

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

المردود 62.1%

المذيبات

methanol

DMSO

ظروف التفاعل

المعالجة

1. 1
   أخرىprepared from the product
2. 2
   أخرىfollowed by evaporation of the solvent]
3. 3
   workup.ADDITIONthen poured onto water (500 ml) and diethylether (250 ml)
4. 4
   workup.ADDITIONwas added
5. 5
   workup.STIRRINGthe solution was stirred for 30 min
6. 6
   أخرىThe layers were separated
7. 7
   درجة الحرارةcooled to 0° C. for 1 h
8. 8
   ترشيحThe precipitated product was filtered off
9. 9
   غسيلwashed with water and diethylether
10. 10
    أخرىdried

الإجراء التجريبي

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+);

المصدر