تفاعل #3235

معادلة التفاعل

7-chloro-2,3-dihydro-10-hydrazinopyridazino[4,5-b]quinoline-1,4-dione hydrochloride

7-Chloro-2,3-dihydro-10-hydrazinopyridazino[4,5-b]quinoline-1,4-dione hydrochloride

beta alanine ethyl ester hydrochloride

→

ester

المردود 13.0%

10-(2-Ethoxycarbonylethylamino)-7-chloro-2,3-dihydropyridazino[4,5-b]quinoline-1,4-dione

المردود 13.0%

المذيبات

water

pyridine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for 23 hr
2. 2
   درجة الحرارةAfter cooling
3. 3
   أخرىthe vigorously stirred reaction mixture
4. 4
   ترشيحfiltered
5. 5
   أخرىto separate a fine red solid
6. 6
   غسيلThe collected solids were washed with water
7. 7
   أخرىchromatographed (eluant: methanol/methylene chloride; 5/95) over silica gel

الإجراء التجريبي

A mixture of 7-chloro-2,3-dihydro-10-hydrazinopyridazino[4,5-b]quinoline-1,4-dione hydrochloride (1.0 g, 2.9 mM, as prepared in Example 44) and beta alanine ethyl ester hydrochloride (49.0 g, 320 mM) in pyridine (52 mL) was refluxed for 23 hr. After cooling, the vigorously stirred reaction mixture was diluted slowly with water (100mL) and then filtered to separate a fine red solid. The collected solids were washed with water and chromatographed (eluant: methanol/methylene chloride; 5/95) over silica gel to provide the title ester (0.13 g, 13%) as a red powder, mp 258°-260° C.; MS(CI): 363 (M+H).

المصدر