반응 #76734

반응 방정식

Potassium tert-butylate

5-(4-ethoxy-1H-indol-6-ylmethyl)-pyrimidine-2,4-diamine

dimethylsulfamoyl chloride

→

title compound

수율 53.0%

6-(2,4-Diamino-pyrimidin-5-ylmethyl)-4-ethoxy-indole-1-sulfonic Acid dimethylamide

수율 53.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.DISTILLATIONafter 30 min the solvent was distilled off
2. 2
   기타the residue partitioned between ethyl acetate and saturated aqueous sodium hydrogencarbonate solution
3. 3
   세척The organic layer was washed with brine
4. 4
   건조dried (MgSO4)
5. 5
   기타evaporated
6. 6
   workup.ADDITIONSuspension of the residue in ether
7. 7
   기타collection of the precipitate

실험 절차

Potassium tert-butylate (42 mg, 0.37 mmol) was added to a solution of 5-(4-ethoxy-1H-indol-6-ylmethyl)-pyrimidine-2,4-diamine (Example 1; 100 mg, 0.353 mmol) in N,N-dimethylformamide (5 mL). After 15 min dimethylsulfamoyl chloride (53 mg, 0.37 mmol) was added, then after 30 min the solvent was distilled off and the residue partitioned between ethyl acetate and saturated aqueous sodium hydrogencarbonate solution. The organic layer was washed with brine, dried (MgSO4), and evaporated. Suspension of the residue in ether and collection of the precipitate afforded the title compound (73 mg, 53%). Off-white solid.

출처