Pyrrolidine → Dimethyl 3,4-Dihydro-2,2-dimethyl-4-oxo-2H-1-benzopyran-6,7-dicarboxylate

HRID 36873ノート

反応式

HRID 36873 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([C:15]([O:17][CH3:18])=[O:16])[C:7](=[CH:12][C:13]=1[OH:14])[C:8]([O:10][CH3:11])=[O:9])(=[O:3])[CH3:2].N1C[CH2:22][CH2:21][CH2:20]1>CC(C)=O>[CH3:20][C:21]1([CH3:22])[CH2:2][C:1](=[O:3])[C:4]2[CH:5]=[C:6]([C:15]([O:17][CH3:18])=[O:16])[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:12][C:13]=2[O:14]1

参加物

4

反応物 2

HCID 31268PyrrolidineHCID 13227611Dimethyl 4-acetyl-5-hydroxyphthalate

生成物 1

HCID 19936389Dimethyl 3,4-Dihydro-2,2-dimethyl-4-oxo-2H-1-benzopyran-6,7-dicarboxylate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

In 100 ml of acetone was dissolved 4.2 g of dimethyl 4-acetyl-5-hydroxyphthalate synthesized in accordance with the process of Bulletin of the Chemical Society of Japan, Vol. 57, p. 3221 (1984). To the solution were added 1.0 ml of pyrrolidine and a small amount of Molecular Sieve (3A), followed by stirring at room temperature for 3 days. Any insoluble material was removed by filtration, and the solvent was removed by distillation under reduced pressure. The residue was purified by silica gel column chromatography to obtain 4.6 g (86.3%) of a yellow oily substance.

後処理

  1. customsynthesized in accordance with the process of Bulletin of the Chemical Society of Japan, Vol. 57, p
  2. customAny insoluble material was removed by filtration
  3. customthe solvent was removed by distillation under reduced pressure
  4. customThe residue was purified by silica gel column chromatography
  5. customto obtain 4.6 g (86.3%) of a yellow oily substance

出典と根拠

ORDレコード
ord-6f7e69cbea9b4ca2a006d71718374361
出典データセット
uspto-grants-1995_05
特許番号
US05418232

反応ノート

読み込み中…