تفاعل #332743

معادلة التفاعل

7-chloro-6-((2R,6S)-2,6-dimethylmorpholino)-3-(pyrazin-2-yl)benzo[d]isoxazole-5-carbaldehyde

Intermediate 472

7-chloro-6-((2R,6S)-2,6-dimethylmorpholino)-3-(pyrazin-2-yl)benzo[d]isoxazole-5-carbaldehyde

pyrimidine-2,4,6(1H,3H,5H)-trione

→

(2R,4S,4aS)-rel-11-chloro-2,4-dimethyl-8-(pyrazin-2-yl)-2,4,4a,6-tetrahydro-1H,1′H-spiro[isoxazolo[4,5-g][1,4]oxazino[4,3-a]quinoline-5,5′-pyrimidine]-2′,4′,6′(3′H)-trione

المذيبات

Isopropanol

ظروف التفاعل

المعالجة

1. 1
   أخرىto give a yellow slurry
2. 2
   درجة الحرارةThe resulting off-white suspension cooled to room temperature
3. 3
   ترشيحfiltered
4. 4
   غسيلThe filtercake was washed with MeOH/hexanes
5. 5
   أخرىto give a white solid, 171 mg (67%)

الإجراء التجريبي

Isopropanol (10 ml) was added to 7-chloro-6-((2R,6S)-2,6-dimethylmorpholino)-3-(pyrazin-2-yl)benzo[d]isoxazole-5-carbaldehyde (Intermediate 472, 198 mg, 0.53 mmol) to give a yellow slurry. The pyrimidine-2,4,6(1H,3H,5H)-trione (barbituric acid) (68.0 mg, 0.53 mmol) was added and the yellow mixture was heated to 80° C. The resulting solution was stirred overnight. The resulting off-white suspension cooled to room temperature, then filtered. The filtercake was washed with MeOH/hexanes to give a white solid, 171 mg (67%).

المصدر