3-Bromopropionic acid → HCID 89377411、化合物
反応式
[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]=1参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-85371d4e8ed847528cc3a12b83fb546c
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09005670B2
反応ノート
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