Dimethylformamide → Methyl pyrrole-2-carboxylate
反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([OH:8])=[O:7].[CH3:9]N(C=O)C.C(N(C(C)C)C(C)C)C.CI>O.C(OCC)(=O)C>[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([O:8][CH3:9])=[O:7]参加物
7
実験手順
To pyrrole-2-carboxylic acid (1.11 g., 0.010 mol) in 5 ml. DMF at 0° was added N-(ethyl)diisopropylamine (1.806 ml., 0.0105 mol) followed by methyl iodide (0.654 ml., 0.0105 mol). The mixture was stirred 18 hours at room temperature, diluted with 10 ml. ethyl acetate and 10 ml. H2O, the pH adjusted to 8.5, and the organic layer separated, washed 1×10 ml. H2O, dried over Na2SO4, and stripped with CHCl3 chase to yield title product as a gummy solid containing 10% DMF, 0.93 g.; 1H-nmr (CDCl3) delta (narrow product peaks only): 3.80 (s, 3H), 6.15 (m, 1H), 6.83 (m, 2H).
後処理
- additiondiluted with 10 ml
- customthe organic layer separated
- washwashed 1×10 ml
- dry with materialH2O, dried over Na2SO4
出典と根拠
- ORDレコード
- ord-572ef2f39fcd48d0b00a5f8adfb2462a
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04762921
反応ノート
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