反応 #10342

反応方程式

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

収率 62.1%

溶媒

methanol

DMSO

反応条件

後処理

1. 1
   その他prepared from the product
2. 2
   その他followed 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
   その他The layers were separated
7. 7
   温度cooled to 0° C. for 1 h
8. 8
   ろ過The precipitated product was filtered off
9. 9
   洗浄washed with water and diethylether
10. 10
    その他dried

実験手順

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+);

出典