تفاعل #46303

معادلة التفاعل

11-(3-chloro-4-fluorobenzyl)-9-methoxy-2-methyl-5,6,12,13-tetrahydro-2H[1,4]diazocino[2,1-a]-2,6-naphthyridine-1,4,8,10(3H, 1H)-tetrone

pyrrolidine

acetic acid

sodium borohydride

→

title compound

11-(3-Chloro-4-fluorobenzyl)-4-pyrrolidin-1-yl-9-methoxy-2-methyl-3,4,5,6,12,13-hexahydro-2H[1,4]diazocino[2,1-a]-2,6-naphthyridine-1,8,10(11H)-trione

المذيبات

dichloroethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled to room temperature
2. 2
   غسيلwashed successively with aq sodium carbonate and brine
3. 3
   استخلاصThe organic extract
4. 4
   تجفيفwas dried over anhydrous magnesium sulfate
5. 5
   ترشيحfiltered
6. 6
   تركيزconcentrated under vacuum

الإجراء التجريبي

A mixture of 11-(3-chloro-4-fluorobenzyl)-9-methoxy-2-methyl-5,6,12,13-tetrahydro-2H[1,4]diazocino[2,1-a]-2,6-naphthyridine-1,4,8,10(3H, 1H)-tetrone (30 mg, 0.06 mmol), molecular sieves (4A), pyrrolidine (23 mg, 0.32 mmol), and acetic acid (4 mg) in dichloroethane (1 mL) was heated at 80° C. for four hrs. The mixture was cooled to room temperature, treated with sodium borohydride (12 mg, 0.19 mmol), and stirred at room temperature for 30 minutes. The product mixture was diluted with dichloromethane, washed successively with aq sodium carbonate and brine. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum to provide the title compound. This material was used in the following step without further purification.

المصدر