Phenobarbital → 5-Ethyl-6-hydroxy-3-(4-methoxycarbonylbutyl)-5-phenyl-2,4(3H,5H)-pyrimidinedione

HRID 1450141

반응식

HRID 1450141 반응식
[CH3:1][CH2:2][C:3]1([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:10](=[O:11])[NH:9][C:7](=[O:8])[NH:6][C:4]1=[O:5].[OH-].C([N+](CCCC)(CCCC)CCCC)CCC.Br[CH2:37][CH2:38][CH2:39][CH2:40][C:41]([O:43][CH3:44])=[O:42].[Cl-].[Na+]>ClCCl>[CH2:2]([C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:10]([OH:11])=[N:9][C:7](=[O:8])[N:6]([CH2:37][CH2:38][CH2:39][CH2:40][C:41]([O:43][CH3:44])=[O:42])[C:4]1=[O:5])[CH3:1]

참가 물질

6

반응물 4

HCID 4763PhenobarbitalHCID 5234Sodium ChlorideHCID 79557Methyl 5-bromovalerateHCID 2723671Tetrabutylammonium Hydroxide

생성물 1

HCID 1784352455-Ethyl-6-hydroxy-3-(4-methoxycarbonylbutyl)-5-phenyl-2,4(3H,5H)-pyrimidinedione

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of phenobarbital (46.5 g, 0.2 mole) and tetrabutylammonium hydroxide (500 mL, 0.2 mole of 0.4M in water) in dichloromethane (500 mL) was prepared and to it was added methyl 5-bromovalerate (39.0 g, 0.2 mole). The reaction mixture was stirred vigorously overnight (20 hrs). To this mixture was added saturated sodium chloride solution (100 mL), the organic layer was separated, and the aqueous solution was washed with dichloromethane (2×100 mL). The combined organic solution was washed with saturated sodium chloride solution (100 mL), dried over anhydrous MgSO4, filtered, and the solvent removed.

후처리

  1. customwas prepared and to it
  2. customthe organic layer was separated
  3. washthe aqueous solution was washed with dichloromethane (2×100 mL)
  4. washThe combined organic solution was washed with saturated sodium chloride solution (100 mL)
  5. dry with materialdried over anhydrous MgSO4
  6. filtrationfiltered
  7. customthe solvent removed

출처 및 근거

ORD 기록
ord-8952355646a94cbca3eb341036e71988
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05601994

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