HRID461446

反应详情

EQUATION

反应方程式

HRID 461446 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Phenyl-2,3-naphthalenedicarboxylic anhydride (VII) (25 g) was added to lithium aluminium hydride (10.4 g) in refluxing tetrahydrofuran (500 ml) over 30 min. and the reactants were refluxed for a further 1 hr. Water was added and the precipitate formed was filtered off and washed with ether (3 × 500 ml). The filtrate and the combined ether washings were dried (Mg2SO4) and evaporated to dryness. The residue was recrystallised from toluene to give 1-phenyl-2,3-bis(hydroxymethyl)naphthalene (VIII) m.p. 150°.

WORKUP

后处理

  1. temperaturethe reactants were refluxed for a further 1 hr
  2. customthe precipitate formed
  3. filtrationwas filtered off
  4. washwashed with ether (3 × 500 ml)
  5. dry with materialThe filtrate and the combined ether washings were dried (Mg2SO4)
  6. customevaporated to dryness
  7. customThe residue was recrystallised from toluene