Sodium Hydroxide → HCID 59301265, Verbindung

Temperatur

150 °C

2-phenyl-2H-benzotriazole (1.10 g, 5.1 mmol) was placed in a 1-neck 250-mL round bottomed flask. HBr/acetic acid (45% w/v, 20 mL) and bromine (0.79 mL, 15.3 mmol) were added. The flask was connected to a condenser and a scrubber. The mixture was heated in an oil bath at 150° C. for 0.5 hr. The solution was cooled to room temperature. Bromine (0.79 mL, 15.3 mmol) was again added to the reaction mixture and it was again heated to 150° C. for 1 hr. This step was repeated three more times. Water (200 mL) and dichloromethane (200 mL) were added to the reaction mixture followed by aqueous sodium hydroxide (1.5 M) solution to neutralize the acid. The organic layer was separated and dried with MgSO4. The solution was filtered and the solvent concentrated using a rotary evaporator. The solid was further dried under high vacuum at 60° C. for 2 hr. Yield: 78%.

1. customThe flask was connected to a condenser
2. temperatureThe solution was cooled to room temperature
3. temperaturewas again heated to 150° C. for 1 hr
4. customThe organic layer was separated
5. dry with materialdried with MgSO4
6. filtrationThe solution was filtered
7. concentrationthe solvent concentrated
8. customa rotary evaporator
9. customThe solid was further dried under high vacuum at 60° C. for 2 hr

ORD-Eintrag

ord-551e446261e548cdbeab5520f7647fac

Quelldatensatz

uspto-grants-2010_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07714099B2