HRID261958

反应详情

EQUATION

反应方程式

HRID 261958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere and at -60° C., 38 ml. (0.08 mol) of a butyllithium solution (20% in n-hexane) were added drop-wise over the course of 45 minutes to a mixture of 9.6 g. (0.08 mol) of N,N,N',N'-tetramethylethylenediamine and 7 g. (0.06 mol) of 1-(methoxymethyl)imidazole in 100 ml. of anhydrous tetrahydrofuran. The mixture was stirred for another two hours under the same conditions and then 16 g (0.0675 mol) of o-tert.-butylbenzophenone in 100 ml. of anhydrous tetrahydrofuran were added dropwise. After the addition was completed, the mixture was stirred for 2 hours at -60° C., and one hour at room temperature. The mixture was decomposed with 5 ml. of water, the precipitate was filtered off and the filtrate was dried over sodium sulphate and concentrated. The solid residue was crystallised from isopropyl alcohol. α-(o-tert.-Butylphenyl)-1-(methoxymethyl)-α-phenylimidazole-2-methanol was obtained. Melting point 149°-150° C.

WORKUP

后处理

  1. customat -60° C.
  2. additionto a mixture of 9.6 g
  3. additionAfter the addition
  4. stirringthe mixture was stirred for 2 hours at -60° C.
  5. customone hour
  6. customat room temperature
  7. filtrationof water, the precipitate was filtered off
  8. dry with materialthe filtrate was dried over sodium sulphate
  9. concentrationconcentrated
  10. customThe solid residue was crystallised from isopropyl alcohol