Dimedone → 5-(4,6-Dimethoxypyrimidin-2-yl)oxy-3-ethylthiocarbonyl-2-methylbenzofuran-4-carboxylic Acid

HRID 52007

반응식

HRID 52007 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[C:25]([C:26]([O:28]CC=C)=[O:27])=[C:16]3[C:17]([C:21]([CH2:23][CH3:24])=[S:22])=[C:18]([CH3:20])[O:19][C:15]3=[CH:14][CH:13]=2)[N:4]=1.CC1(C)CC(=O)CC(=O)C1>O1CCCC1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[C:25]([C:26]([OH:28])=[O:27])=[C:16]3[C:17]([C:21]([CH2:23][CH3:24])=[S:22])=[C:18]([CH3:20])[O:19][C:15]3=[CH:14][CH:13]=2)[N:4]=1

참가 물질

4

반응물 2

HCID 31358DimedoneHCID 53832981Allyl 5-(4,6-dimethoxypyrimidin-2-yl)oxy-3-ethylthiocarbonyl-2-methylbenzofuran-4-carboxylate

생성물 1

HCID 544680195-(4,6-Dimethoxypyrimidin-2-yl)oxy-3-ethylthiocarbonyl-2-methylbenzofuran-4-carboxylic Acid수율 91.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1.60 g of allyl 5-(4,6-dimethoxypyrimidin-2-yl)oxy-3-ethylthiocarbonyl-2-methylbenzofuran-4-carboxylate and 0.54 g of dimedone were dissolved in 14 ml of tetrahydrofuran, and 40 mg of tetrakistriphenylphosphine palladium (0) was added thereto under a nitrogen atmosphere. The mixture was stirred at room temperature for 3 hours. The reaction solution was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=2/1) to obtain 1.33 g (yield: 91%) of the desired compound.

후처리

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=2/1)

출처 및 근거

ORD 기록
ord-20301908661145a2bcc9f8c17eecf4a7
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616537

연결된 노트

불러오는 중…