반응 #218959

ord-db3240e846d947fe850b42518ed511a3

반응 방정식

CCCCCCC(C)O
2-octanol
Cc1ccc(S(=O)(=O)O)cc1.O
p-toluenesulfonic acid monohydrate
c1ccc2c(c1)Nc1ccccc1S2
phenothiazine
C=CC(=O)OC(C)CCCCCC
product
C=CC(=O)OC(C)CCCCCC
2-octyl acrylate

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated to reflux
  2. 2
    기타Water was separated from the toluene/water
  3. 3
    workup.DISTILLATIONa Dean Stark distillation trap
  4. 4
    온도After six hours at reflux a total of 37 milliliters of water
  5. 5
    기타was collected in the trap
  6. 6
    세척The reaction mixture was washed with 1 Molar aqueous sodium hydroxide (200 milliliters)
  7. 7
    농축concentrated under reduced pressure
  8. 8
    workup.DISTILLATIONThe remaining oil was distilled under reduced pressure (65-67° C. at 2 mmHg)

실험 절차

A mixture of 2-octanol (268.51 grams, 2.1 mol), AA (183.75 grams, 2.6 mol), p-toluenesulfonic acid monohydrate (5.00 grams, 26 mmol), toluene (250 grams) and phenothiazine (1.0 grams) was heated to reflux. Water was separated from the toluene/water azeotrope using a Dean Stark distillation trap. After six hours at reflux a total of 37 milliliters of water was collected in the trap. The reaction mixture was washed with 1 Molar aqueous sodium hydroxide (200 milliliters), then concentrated under reduced pressure. The remaining oil was distilled under reduced pressure (65-67° C. at 2 mmHg) to give the product as a colorless oil. (Yield: 248.6 grams)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07385020B2uspto-grants-2008_06