反应 #1605781

ord-eb35be541a3348da85d034c40f8d7de8

反应方程式

Cc1ccc(N=C=O)cc1
para-tolylisocyanate
Cc1ccccc1
toluene
CC(C)C1CCCCC1O
2-isopropylcyclohexanol
Cc1ccc(NC(=O)OC2CCCCC2C(C)C)cc1
product
收率 56.8%
Cc1ccc(NC(=O)OC2CCCCC2C(C)C)cc1
p-Tolyl-carbamic acid 2-isopropyl-cyclohexyl ester
收率 56.8%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was heated
  2. 2
    温度to reflux for 6 hours
  3. 3
    workup.ADDITIONwere added
  4. 4
    温度the mixture was refluxed for one more hour
  5. 5
    其他After phase separation the solvent
  6. 6
    其他the crude product recrystallized from 235 g of n-heptane

实验过程

75.6 g (0.56 mol) of para-tolylisocyanate were placed with 500 ml toluene in a one litre vessel and subsequently 73.4 g (0.51 mol) of 2-isopropylcyclohexanol were added. The reaction mixture was heated to reflux for 6 hours. After cooling to room temperature 50 g of water were added and the mixture was refluxed for one more hour. After phase separation the solvent was stripped off and the crude product recrystallized from 235 g of n-heptane. The product (79.8 g) was obtained in form of off-white crystals in 99.2% purity. This corresponds to a theoretical yield of 56%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09072676B2uspto-grants-2015_07