Urea → HCID 178487639, Verbindung

Temperatur

175 °C

2-Formyl-5-methoxyaniline (11.93 g, 79.5 mmol, 1.0 eq) and urea (38.0 g, 0.636 mol, 8.0 eq) were mixed, ground into a fine powder and placed into a 1 L 2-neck flask equipped with a mechanical stirrer and an air condenser. The flask was placed into a preheated (160° C.) oil bath. The reaction mixture melted and was stirred at 170-180° C. for 1 hour until it solidified forming yellowish-brown solid. The reaction mixture was cooled to RT, crushed, mixed with 70 mL of H2O and stirred for ˜1 hour at RT. The solid was filtered, washed with 150 mL of H2O and 20 mL of ice cold Et2O. The yellow solid thus obtained was dried over P4O10 under high vacuum for several hours and the crude material (12.57 g) was used for the next step without purification.

1. customequipped with a mechanical stirrer and an air condenser
2. customwas placed into a preheated (160° C.) oil bath
3. customsolidified forming yellowish-brown solid
4. temperatureThe reaction mixture was cooled to RT
5. customcrushed
6. stirringstirred for ˜1 hour at RT
7. filtrationThe solid was filtered
8. washwashed with 150 mL of H2O and 20 mL of ice cold Et2O
9. customThe yellow solid thus obtained
10. dry with materialwas dried over P4O10 under high vacuum for several hours
11. customthe crude material (12.57 g) was used for the next step without purification

ORD-Eintrag

ord-e53372179d344de9a4355461e84c14f5

Quelldatensatz

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07932262B2