تفاعل #62058

معادلة التفاعل

2

5,5-Dichloro-1-morpholin-4-yl-pent-4-ene-1,3-dione

perchloric acid

NaOH

→

3

المردود 75.4%

2-Chloro-6-morpholin-4-yl-pyran-4-one

المردود 75.4%

المذيبات

dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction was cooled
2. 2
   ترشيحfiltered
3. 3
   استخلاصThe aqueous layer was extracted with DCM (4×30 ml)
4. 4
   تجفيفdried over MgSO4
5. 5
   workup.ADDITIONThe organic layer was further treated with charcoal
6. 6
   ترشيحfiltered through celite
7. 7
   أخرىThe dark yellow filtrate was evaporated in vacuo
8. 8
   أخرىthe resulting solid was triturated with hexane (50 ml)
9. 9
   أخرىdried

الإجراء التجريبي

To a suspension of 2 (11.3 g, 44.9 mmol) in dioxane was added perchloric acid (11.4 ml, 0.14 mol) and the reaction was heated at 90° C. under N2 for 1 hour. The reaction was cooled, neutralised with 2M NaOH (75 ml) and filtered. The aqueous layer was extracted with DCM (4×30 ml) and the organic layers were combined and dried over MgSO4. The organic layer was further treated with charcoal and filtered through celite. The dark yellow filtrate was evaporated in vacuo, and the resulting solid was triturated with hexane (50 ml) and dried to give 3 (7.3 g, 75%) as a light yellow powder. m/z (LC-MS, ESP): 216 (M++1). 1H-NMR (300 MHz, DMSO-d6): 3.3 (t, 4H), 3.65 (t, 4H), 5.4 (d, 1H), 6.25 (d, 1H).

المصدر