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

HRID 36873노트

반응식

HRID 36873 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f7e69cbea9b4ca2a006d71718374361
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418232

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