Potassium Hydroxide → 3-Acetyl-4,5-dimethyl-1H-pyrrole-2-carboxylic acid
反応式
C([O:3][C:4]([C:6]1[NH:7][C:8]([CH3:15])=[C:9]([CH3:14])[C:10]=1[C:11](=[O:13])[CH3:12])=[O:5])C.[OH-].[K+]>C(O)C>[C:11]([C:10]1[C:9]([CH3:14])=[C:8]([CH3:15])[NH:7][C:6]=1[C:4]([OH:5])=[O:3])(=[O:13])[CH3:12]参加物
4
実験手順
A mixture of pyrrole ester 34 (8.2 g, 0.0392 mol), in ethanol and 100 mL of 10% potassium hydroxide were refluxed for 1 h. The mixture was cooled and concentrated in vacuo to an oil. Water was added to the oil, the mixture acidified with dilute HCl and extracted with ether. The organic phase was dried with anhy. sodium sulfate and concentrated in vacuo to a solid residue. The compound was recrystallized in 80 mL of ethanol to give 5.8 g of pure 3-acetyl-4,5-dimethyl-2-pyrrole carboxylic acid 35 as a solid. 1H NMR (DMSO-d6) δ 2.5 (s, 3H), 2.2 (s, 3H), 2.0 (s, 3H) ppm.
後処理
- temperatureThe mixture was cooled
- concentrationconcentrated in vacuo to an oil
- additionWater was added to the oil
- extractionextracted with ether
- customThe organic phase was dried with anhy
- concentrationsodium sulfate and concentrated in vacuo to a solid residue
- customThe compound was recrystallized in 80 mL of ethanol
出典と根拠
- ORDレコード
- ord-2274a5ab22434a2da0e693ffa79854ab
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07906550B2
反応ノート
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