تفاعل #2392588

معادلة التفاعل

(1S,4S)-(5-pyrimidinyl)-2,5-diazabicyclo[2.2.1]heptane

mucic acid

→

white solid

المردود 59.4%

(1S,4S)-(5-Pyrimidinyl)-2,5-diazabicyclo[2.2.1]heptane hemigalactarate

المردود 59.4%

المذيبات

methanol

water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   درجة الحرارةThe mixture was heated for 30 min.
3. 3
   ترشيحthen filtered through glass wool
4. 4
   تركيزconcentrated to approximately 1 mL
5. 5
   workup.ADDITIONThe treated with diethyl ether (5 mL)
6. 6
   أخرىthe precipitate was collected
7. 7
   غسيلwashed with diethyl ether (1 mL)
8. 8
   أخرىdried at 45° C. for 4 h

الإجراء التجريبي

A solution of (1S,4S)-(5-pyrimidinyl)-2,5-diazabicyclo[2.2.1]heptane (0.15 g, 0.851 mmol) in methanol (3 mL) and water (3 mL) was heated at 60° C. as mucic acid (0.09 g, 0.425 mmol) was added. The mixture was heated for 30 min. then filtered through glass wool and concentrated to approximately 1 mL. The treated with diethyl ether (5 mL), then the precipitate was collected, washed with diethyl ether (1 mL) and dried at 45° C. for 4 h to afford (0.142 g, 59%) of white solid, mp 152-172° C. (d).

المصدر