تفاعل #2006477

معادلة التفاعل

compound 4a

4-[4,4-dimethyl-3-(3-hydroxypropyl)-5-imino-2-thioxo-1-imidazolidinyl]-2-trifluoromethyl-benzonitrile

hydrogen chloride

methanol

→

desired compound 5a

المردود 68.0%

4-[4,4-dimethyl-3-(3-hydroxypropyl)-5-oxo-2-thioxo-1-imidazolidinyl]-2-trifluoromethyl-benzonitrile

المردود 68.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution was refluxed for 90 min
2. 2
   استخلاصThe solution was extracted with ethyl acetate (3×30 mL)
3. 3
   غسيلwashed with brine
4. 4
   تجفيفdried over magnesium sulphate

الإجراء التجريبي

To a solution of compound 4a (627 mg, 1.7 mmol) in methanol (27 mL) was added 2N aqueous hydrogen chloride (5.2 mL). The solution was refluxed for 90 min and then poured in an ice/water solution. The solution was extracted with ethyl acetate (3×30 mL), washed with brine, and dried over magnesium sulphate to give 428 mg (68%) of desired compound 5a. 1H NMR (400 MHz, Acetone-d6) δ: 1.65 (s, 6H), 3.67 (q, 2H, J=5.7 Hz), 3.75 (t, 1H, J=5.01 Hz), 3.90 (m, 2H), 8.03 (d, 1H, J=6.4 Hz), 8.18 (s, 1H), 8.26 (d, 1H, J=8.26 Hz).

المصدر