Sodium Carbonate → 5-Hydroxy-2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)-6-methyl-nicotinic acid methyl ester

HRID 329429노트

반응식

HRID 329429 반응식
[CH3:1][O:2][C:3](=[O:26])[C:4]1[CH:9]=[C:8]([O:10]C(=O)C)[C:7]([CH3:14])=[N:6][C:5]=1[C:15](=O)[NH:16][C:17]([C:22](=[O:24])[NH2:23])([CH3:21])[CH:18]([CH3:20])[CH3:19].P(Cl)(Cl)(Cl)(Cl)Cl.C(=O)([O-])[O-].[Na+].[Na+]>O=P(Cl)(Cl)Cl>[CH3:1][O:2][C:3](=[O:26])[C:4]1[CH:9]=[C:8]([OH:10])[C:7]([CH3:14])=[N:6][C:5]=1[C:15]1[NH:23][C:22](=[O:24])[C:17]([CH:18]([CH3:20])[CH3:19])([CH3:21])[N:16]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 24819Phosphorus pentachlorideHCID 137994465-Acetoxy-2-(1-carbamoyl-1,2-dimethylpropyl-carbamoyl)-6-methyl-nicotinic acid methyl ester

생성물 1

HCID 1363428005-Hydroxy-2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)-6-methyl-nicotinic acid methyl ester

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

A solution of 47 g (0.129 mol) 5-acetoxy-2-(1-carbamoyl-1,2-dimethylpropyl-carbamoyl)-6-methyl-nicotinic acid methyl ester and 93.8 g phosphorus pentachloride in 470 ml phosphoroxychloride is stirred 12 hours at room temperature. The solution is then hydrolysed with ice and neutralized with sodium carbonate. The product is extracted with ethyl acetate, the extract is then dried across magnesium sulfate and compressed. The crude product is recrystallized from ethyl acetate/isopropyl ester.

후처리

  1. extractionThe product is extracted with ethyl acetate
  2. dry with materialthe extract is then dried across magnesium sulfate
  3. customThe crude product is recrystallized from ethyl acetate/isopropyl ester

출처 및 근거

ORD 기록
ord-a39d1e917e664c3bb1f12678f59852d6
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04891428

반응 노트

불러오는 중…