تفاعل #696708

ord-403eb750e145455fa6b509654d3dcc42

معادلة التفاعل

CC(C)(C)c1ccc(O)c([N+](=O)[O-])c1
nitrophenol
CC(C)(C)c1ccc(O)c([N+](=O)[O-])c1
2-nitro-4-t-butyl phenol
[H][H]
hydrogen
CC(C)(C)c1ccc(O)c(N)c1
amine
المردود 81.5%

الكواشف

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe catalyst was filtered off through celite
  2. 2
    أخرىThe material crystallized with the addition of about 200 mL heptane

الإجراء التجريبي

Commercially available 4-t-butyl phenol (30 g, 0.2 mole) was dissolved in 200 mL ethyl acetate in a 600-mL round-bottomed flask fitted with a mechanical stirrer, and cooled to 0° C. The mixture was treated with nitric acid (13 mL, in 13 mL water) dropwise over 10 min and then a catalytic amount of NaNO2. After 45 min the reaction was washed with excess 1N HCl and the organic layer was dried over MgSO4 and stripped to yield 37 g of 2-nitro-4-t-butyl phenol. This nitrophenol (37 g, 0.19 mole) was dissolved in 100 mL ethyl acetate and placed into a Parr bottle with a teaspoon of 10% Pd/C. The mixture was placed on a hydrogenator under 50 psi hydrogen with agitation for 1 hr. The catalyst was filtered off through celite, and the ethyl acetate was stripped off under vacuum. The material crystallized with the addition of about 200 mL heptane to give 25.6 g of the corresponding amine (2-amino-4-t-butyl phenol).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05998121uspto-grants-1999_12