반응 #1605781

ord-eb35be541a3348da85d034c40f8d7de8

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was heated
  2. 2
    온도to reflux for 6 hours
  3. 3
    workup.ADDITIONwere added
  4. 4
    온도the mixture was refluxed for one more hour
  5. 5
    기타After phase separation the solvent
  6. 6
    기타the crude product recrystallized from 235 g of n-heptane

실험 절차

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%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09072676B2uspto-grants-2015_07