반응 #90997

ord-74e0c5cb1e9943aa826529780e22bf7a

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was partitioned between EtOAc and water
  2. 2
    추출the aqueous phase was extracted twice with EtOAc
  3. 3
    세척The combined organic phases were washed with brine
  4. 4
    건조dried over MgSO4
  5. 5
    여과filtered
  6. 6
    기타the solvent removed in vacuo

실험 절차

Ethanol (20 mL, 343 mmol) was treated with potassium hydroxide (956 mg, 17.0 mmol) and the mixture was stirred at RT for 1 h. A solution of 2-chloro-5-nitro-1,3-bis(trifluoromethyl)benzene (1) (1.00 g, 3.41 mmol) in DMSO (10 mL) was added dropwise. The resultant mixture was stirred at RT for 1 h. The mixture was partitioned between EtOAc and water and the aqueous phase was extracted twice with EtOAc. The combined organic phases were washed with brine, dried over MgSO4, filtered and the solvent removed in vacuo to afford 2-ethoxy-5-nitro-1,3-bis(trifluoromethyl)benzene (2) (1.00 g, 93%) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ: 8.72 (2H, s), 4.21 (2H, q), 1.41 (3H, t).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447028B2uspto-grants-2016_09