반응 #159254

ord-c027ee709fac4a838a7b3ef6f1a06eef

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도a thermometer a “wood metal” heating bath and a reflux condenser
  2. 2
    기타had separated (about 4 hours)
  3. 3
    workup.ADDITIONWhen cold, 50 ml of diisopropylether were added
  4. 4
    여과this mixture was filtered
  5. 5
    세척the crystalline product was washed with diisopropylether and pentane
  6. 6
    기타dried

실험 절차

A 350 ml three necked reaction flask, equipped with a mechanical stirrer, a thermometer a “wood metal” heating bath and a reflux condenser combined with a water separator were charged with 25.1 g (140 mmol) of 2-amino-4-(1,1-dimethyl-propyl)-phenol (see above), 19.3 g (140 mmol) of 4-hydroxy benzoic acid and 1.5 g of boric acid suspended in 140 ml of 1,2-dichlorobenzene under nitrogen atmosphere. This mixture was refluxed until two equivalents of water had separated (about 4 hours). When cold, 50 ml of diisopropylether were added and this mixture was filtered and the crystalline product was washed with diisopropylether and pentane and dried. 32.1 g (81%) of the product were obtained. M.p. 236-237° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08828365B2uspto-grants-2014_09