Methanol → Methyl 5-oxo-L-prolinate
반응식
[NH:1]1[C:5](=[O:6])[CH2:4][CH2:3][C@H:2]1[C:7]([OH:9])=[O:8].S(Cl)(Cl)=O.[CH3:14]O>>[CH3:14][O:8][C:7](=[O:9])[C@@H:2]1[CH2:3][CH2:4][C:5](=[O:6])[NH:1]1참가 물질
4
반응 조건
- 온도
- 0 °C
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.
후처리
- customThe bath was removed
- stirringstirring
- additionWater (150 mL) and solid NaHCO3 (60 g) were added
- customthe CH3OH was removed on a rotary evaporator
- extractionthe residue extracted with CH2Cl2 (3×150 mL)
- washwashed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated to dryness
출처 및 근거
- ORD 기록
- ord-4d59c37e20d84a41aea1bc6a4182c2d8
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05624936
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