반응 #86500

ord-98472b128ff34c7080db4dbfec015a2b

시약

없음

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at 0° C.
  2. 2
    온도to warm to room temperature overnight
  3. 3
    workup.STIRRINGWhile stirring
  4. 4
    기타a stream of air was bubbled through the solution for 1 hour
  5. 5
    건조The reaction mixture was dried over sodium sulfate
  6. 6
    기타the solvent evaporated under reduced pressure

실험 절차

Under a nitrogen atmosphere, a solution of bromine (8.61 mL, 167 mmol) in chloroform (20 mL) was added drop-wise over a period of 2 h to a solution of methyl 3-oxohexanoate (Fluka, 24.1 g, 167 mmol) in chloroform (147 mL), at 0° C. (ice bath). The reaction mixture was stirred for 30 min at 0° C. and then allowed to warm to room temperature overnight. While stirring, a stream of air was bubbled through the solution for 1 hour. The reaction mixture was dried over sodium sulfate and the solvent evaporated under reduced pressure to provide the desired compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09434746B2uspto-grants-2016_09