반응 #415525

ord-efbfbebf66014f23bbf37360e380f506

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe addition
  2. 2
    기타The excess phosgene and hydrogen chloride are removed with a stream of nitrogen
  3. 3
    기타the residual solution evaporated to dryness in vacuo
  4. 4
    기타affording 17.9 g

실험 절차

20.4 G. (0.2 moles) of 2-ethyl-1-butanol is added dropwise under anhydrous conditions to 250 ml. (0.4 moles) of 17.2% phosgene solution in benzene with stirring in an ice bath. The addition is complete in 70 minutes and the solution is allowed to gradually warm to room temperature and stirred for 16 hours. The excess phosgene and hydrogen chloride are removed with a stream of nitrogen and the residual solution evaporated to dryness in vacuo affording 17.9 g. (54%) of a light yellow oil which IR demonstrates having a strong chloroformate band and no hydroxy. The oil is used as is in further reactions.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04017505uspto-grants-1977_04