反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH:6]=[O:7].[C:8]([O:12][C:13](=[O:16])[CH2:14]Br)([CH3:11])([CH3:10])[CH3:9].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C=O)C>[CH:6]([C:2]1[N:1]([CH2:14][C:13]([O:12][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:16])[CH:5]=[CH:4][N:3]=1)=[O:7]参加物
6
反応条件
- 温度
- 110 °C
実験手順
To a solution of 2-imidazole carboxaldehyde (1.00 g, 10.4 mmol) in DMF (1 mL) was added 1 eq. tert-butylbromoacetate, potassium carbonate and a catalytic amount of potassium iodide. The reactions were heated at 110° C. for 18 hrs followed by evaporation to dryness and purified utilizing a Biotage SP4 with a gradient method of 5-50% methanol in DCM to yield the desired compound (850 mg, 4.03 mmol, 39% yield). 1H NMR (400 MHz, DMSO-d6) δ 7.6 (s, H), 7.23 (s, H), 5.15 (s, 2H), 1.40 (s, 9H).
後処理
- customfollowed by evaporation to dryness
- custompurified
出典と根拠
- ORDレコード
- ord-88839a69102c463f8688f31e81137fb1
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09433594B2
関連ノート
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