Isobutyryl chloride → HCID 178429167、化合物
反応式
[NH2:1][C:2]1[N:7]([NH2:8])[C:6](=[O:9])[CH:5]=[C:4]([CH3:10])[N:3]=1.[C:11](Cl)(=O)[CH:12]([CH3:14])[CH3:13]>O1CCOCC1.CN(C)C=O>[CH3:10][C:4]1[CH:5]=[C:6]([OH:9])[N:7]2[N:8]=[C:11]([CH:12]([CH3:14])[CH3:13])[N:1]=[C:2]2[N:3]=1参加物
5
実験手順
A solution of Intermediate 1 (0.35 g, 2.497 mmol) and iso-butyryl chloride (FLUKA, 0.262 mL, 2.497 mmol) in a mixture of 1,4-dioxane (4 mL) and N,N-dimethylformamide (1 mL) was heated under reflux overnight. The reaction was then concentrated under vacuum and the residue was purified by flash chromatography (Si, eluting with DCM:MeOH mixtures, gradient from 100:0% to 90:10%) to yield the title compound as a white solid.
後処理
- temperaturewas heated
- temperatureunder reflux overnight
- concentrationThe reaction was then concentrated under vacuum
- customthe residue was purified by flash chromatography (Si, eluting with DCM:MeOH mixtures, gradient from 100:0% to 90:10%)
出典と根拠
- ORDレコード
- ord-947b58105c184ffc98d225fe3f7f7908
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09238653B2
反応ノート
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