3-Bromopropionic acid → HCID 89377411, 화합물
반응식
[CH3:1][C:2]1[N:3]=[N:4][C:5](=[O:7])[CH:6]=1.Br[CH2:9][CH2:10][C:11]([OH:13])=[O:12]>O1CCOCC1>[CH3:1][C:2]1[CH2:6][C:5](=[O:7])[N:4]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])[N:3]=1참가 물질
4
실험 절차
To a solution of 3-methyl-pyrazol-5-one (5.7 g, 58.0 mmol) in anhydrous 1,4-dioxane was added 3-bromopropionic acid, and the resulting mixture was heated to reflux for 48 h.12 The reaction mixture was concentrated under reduced pressure, and the crude product was purified by column chromotography using 5-10% MeOH/DCM as an eluent to give 3j (22%) as a solid.13 mp: 210-215° C. (Lit. mp 178-180° C.); 1H NMR (400 MHz, CDCl3): δ 2.21 (s, 3H), 2.76 (m, 2H), 3.14 (s, 2H), 4.14 (m, 2H), 8.01 (brs, 1H); HRMS (m/z): [M−H]− calcd for C7H4N2O3, 169.0619; found, 169.0622.
후처리
- temperaturethe resulting mixture was heated
- temperatureto reflux for 48 h
- concentration12 The reaction mixture was concentrated under reduced pressure
- customthe crude product was purified by column chromotography
출처 및 근거
- ORD 기록
- ord-85371d4e8ed847528cc3a12b83fb546c
- 출처 데이터셋
- uspto-grants-2015_04
- 특허 번호
- US09005670B2
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