3-Hydroxybenzaldehyde → 3-(Oxiran-2-ylmethoxy)benzaldehyde
반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].[H-].[Na+].Br[CH2:13][CH:14]1[CH2:16][O:15]1>CN(C=O)C>[O:15]1[CH2:16][CH:14]1[CH2:13][O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]참가 물질
5
실험 절차
To a solution of 3-hydroxybenzaldehyde (2.0 g, 16.38 mmol) in DMF (30 mL) at 0° C. was added NaH (983 mg, 24.57 mmol) in portions. After 0.5 h, a solution of 2-(bromomethyl)oxirane (2.69 mg, 19.65 mmol) in DMF (5 mL) was added and the reaction mixture was warmed to room temperature for 5 h. The mixture was concentrated, dissolved in ethyl acetate and washed with water. The organic portion was dried over sodium sulfate, filtered and concentrated. The crude product was used in the next step without further purification. (2.1 g, yield 72%) MS (ESI+) e/z: 179.1 [M+1]+.
후처리
- concentrationThe mixture was concentrated
- dissolutiondissolved in ethyl acetate
- washwashed with water
- dry with materialThe organic portion was dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was used in the next step without further purification
출처 및 근거
- ORD 기록
- ord-be67e3b35af34312a7d58b4c3d47ee48
- 출처 데이터셋
- uspto-grants-2015_12
- 특허 번호
- US09221794B2
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