Dimethylformamide → Methyl 1-methylpyrrole-2-carboxylate

HRID 34734

反応式

HRID 34734 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7]([OH:9])=[O:8].[CH3:10]N(C=O)C.C(N(C(C)C)C(C)C)C.CI>C(OCC)(=O)C.O>[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7]([O:9][CH3:10])=[O:8]

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 814531-Methyl-2-pyrrolecarboxylic acidHCID 81531Diisopropylethylamine

生成物 1

HCID 142178Methyl 1-methylpyrrole-2-carboxylate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To 1-methylpyrrole-2-carboxylic acid (28.66 g., 0.229 mol) in 75 ml. DMF at 0° was added N-ethyl diisopropylamine (39.4 ml., 0.229 mol) followed by CH3I (14.27 ml., 0.229 mol). The reaction mixture was stirred 16 hours at room temperature, diluted with equal volumes each of ethyl acetate and water, the pH adjusted from 3.4 to 8.5, and the layers evaporated. The aqueous layer was washed 1×100 ml. fresh ethyl combined, washed 2×100 ml. H2O and 1×100 ml. brine, dried over Na2SO4 and stripped to yield title product as an oil, 24.83 g.; 1H-nmr (CDCl3) delta 3.75 (s, 3H), 3.87 (s, 3H), 5.97 (m, 1H), 6.62 (m, 1H), 6.78 (m, 1H).

後処理

  1. customthe layers evaporated
  2. washThe aqueous layer was washed 1×100 ml
  3. washwashed 2×100 ml
  4. dry with materialbrine, dried over Na2SO4

出典と根拠

ORDレコード
ord-8846fd4203b048b2955171644a99b630
出典データセット
uspto-grants-1988_08
特許番号
US04762921

関連ノート

読み込み中…