반응 #83393

ord-4d59c37e20d84a41aea1bc6a4182c2d8

반응 조건

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

후처리

  1. 1
    기타The bath was removed
  2. 2
    workup.STIRRINGstirring
  3. 3
    workup.ADDITIONWater (150 mL) and solid NaHCO3 (60 g) were added
  4. 4
    기타the CH3OH was removed on a rotary evaporator
  5. 5
    추출the residue extracted with CH2Cl2 (3×150 mL)
  6. 6
    세척washed with brine
  7. 7
    건조dried (MgSO4)
  8. 8
    여과filtered
  9. 9
    농축concentrated to dryness

실험 절차

L-Pyroglutamic acid (15.17 g, 0.1175 mol) was dissolved in CH3OH (100 mL), cooled to 0° C. under Ar and treated dropwise with thionyl chloride (18.9 mL, 0.259 mol) with stirring. The bath was removed and stirring was continued at ambient temperature for 3.5 h. Water (150 mL) and solid NaHCO3 (60 g) were added, the CH3OH was removed on a rotary evaporator, and the residue extracted with CH2Cl2 (3×150 mL). The organic layers were combined, washed with brine, dried (MgSO4), filtered and concentrated to dryness to give the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05624936uspto-grants-1997_04