HRID1730971

反应详情

EQUATION

反应方程式

HRID 1730971 的结构方程式

PROCEDURE

实验过程

A mixture of 10.0 g. of 10,11-dihydro-spiro[dibenzo[a,d] cycloheptene-5,2'-oxirane] and 100 ml. of anhydrous hydrazine is refluxed for 3 hours, the resulting mixture evaporated in vacuo to dryness, the residue dissolved in methanol and again evaporated in vacuo to dryness. The residue is crystallized from diethyl ether to obtain 5-hydrazinomethyl-10,11-dihydro-5H-dibenzo[a,d]cyclo-hepten-5-ol, m.p. 95°-105° C. (decomp.). It was observed that this product decomposed slowly at room temperature to form dibenzo[a,d]cyclohepten-5-one and thus must be stored at reduced temperatures if to be preserved in relatively pure form for any substantial period of time.

WORKUP

后处理

  1. additionA mixture of 10.0 g
  2. customthe resulting mixture evaporated in vacuo to dryness
  3. dissolutionthe residue dissolved in methanol
  4. customagain evaporated in vacuo to dryness
  5. customThe residue is crystallized from diethyl ether