HRID1065587

反应详情

EQUATION

反应方程式

HRID 1065587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Two thousand one hundred and eighty (2,180) grams (2,060 cc) of benzyl alcohol and 1,560 g (1,780 cc) of benzene were introduced into a 10-liter flask, and 940 g of boron trifluoride gas was blown into the flask. The whole mass was transferred into an autoclave, agitated at 60° C. for 9 hours, heated, thereafter cooled and then separated into the lower layer (acid layer) and upper layer (oil layer). The upper layer (oil layer) was incorporated with 1.5 l of a 10% aqueous solution of sodium hydroxide, repeatedly agitated and washed eight times and then distilled to obtain 480 g of a distillate boiling in the range of 173°-176° C. at 72 mm Hg. This distillate had a boiling point of 261° C. at atmospheric pressure, 175° C. at 72 mm Hg, 149° C. at 29 mm Hg or 85° C. at 1 mm Hg, a specific gravity (30/4° C.) of 0.997, a viscosity of 0.01564 g/cm.sec (59° C.) ad a refractive index (nD25) of 1.570, and it was found to be diphenylmethane as the main ingredient from its NMR spectra and gas chromatography. The yield of the diphenylmethane was about 15% (about 460 g), and other distillates having a high boiling point such as dibenzylbenzene and tribenzylbenzene were produced in an amount of 989 g as by-products.

WORKUP

后处理

  1. temperatureheated
  2. temperaturecooled
  3. customseparated into the lower layer (acid layer) and upper layer (oil layer)
  4. stirringrepeatedly agitated
  5. washwashed eight times
  6. distillationdistilled
  7. customto obtain 480 g of a distillate
  8. customboiling in the range of 173°-176° C. at 72 mm Hg
  9. customat atmospheric pressure, 175° C.
  10. customat 72 mm Hg, 149° C.
  11. customat 29 mm Hg or 85° C.
  12. customa specific gravity (30/4° C.) of 0.997
  13. customsec (59° C.) ad