Methanol → 2-(1H-1,2,4-triazol-3-yl)acetic acid
반응식
[NH:1]1[CH:5]=[N:4][C:3]([CH2:6][C:7]([O:9]CC)=[O:8])=[N:2]1.[OH-].[Na+].O.CO>C1COCC1>[NH:1]1[CH:5]=[N:4][C:3]([CH2:6][C:7]([OH:9])=[O:8])=[N:2]1참가 물질
6
반응 조건
- 온도
- 100 °C
실험 절차
A mixture of ethyl 1H-1,2,4-triazol-3-ylacetate obtained in Reference Example 14 (900 mg, 5.80 mmol), 4N aqueous sodium hydroxide solution (7.25 mL, 29.0 mmol), water (10 mL), methanol (10 mL) and THF (10 mL) was stirred at 100° C. for 2 hr. The reaction mixture was concentrated under reduced pressure, the residue was acidified with 1N hydrochloric acid, and the mixture was concentrated under reduced pressure. Ethanol was added to the residue, and the insoluble material was filtered off, and the filtrate was concentrated. The residue was crystallized from toluene to give the title compound as a white powder (369 mg, 50%).
후처리
- concentrationThe reaction mixture was concentrated under reduced pressure
- concentrationthe mixture was concentrated under reduced pressure
- additionEthanol was added to the residue
- filtrationthe insoluble material was filtered off
- concentrationthe filtrate was concentrated
- customThe residue was crystallized from toluene
출처 및 근거
- ORD 기록
- ord-ec4c4f925dda47fb8817c9f10dff6bc8
- 출처 데이터셋
- uspto-grants-2011_03
- 특허 번호
- US07915267B2
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