Phenyl glycidyl ether → YM 16151-1

HRID 4663

반응식

HRID 4663 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=1[CH:16]1[C:21]([C:22]([O:24][CH3:25])=[O:23])=[C:20]([CH3:26])[NH:19][C:18]([CH3:27])=[C:17]1[C:28]([O:30][CH3:31])=[O:29].[C:32]1([O:38][CH2:39][CH:40]2[O:42][CH2:41]2)[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1>CO>[OH:42][CH:40]([CH2:39][O:38][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[CH2:41][NH:1][CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=1[CH:16]1[C:21]([C:22]([O:24][CH3:25])=[O:23])=[C:20]([CH3:26])[NH:19][C:18]([CH3:27])=[C:17]1[C:28]([O:30][CH3:31])=[O:29]

참가 물질

4

반응물 2

HCID 31217Phenyl glycidyl etherHCID 14306630Dimethyl 4-[2-(4-aminobutoxy)-5-nitrophenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate

생성물 1

HCID 128387YM 16151-1수율 51.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 1,300 ml of methanol were dissolved 13 g of dimethyl 4-[2-(4-aminobutoxy)-5-nitrophenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate and 4.5 g of glycidyl phenyl ether, and the solution thus formed was refluxed under heating for 16 hours. The solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography, and the product was eluted with chloroform-methanol (96:4 v/v). Crude crystals were recrystallized from ethanol to give 9 g of dimethyl 4-[2-[4-(2-hydroxy-3-phenoxypropylamino)butoxy]-5-nitrophenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate.

후처리

  1. customthe solution thus formed
  2. temperaturewas refluxed
  3. temperatureunder heating for 16 hours
  4. distillationThe solvent was distilled off under reduced pressure
  5. washthe product was eluted with chloroform-methanol (96:4 v/v)
  6. customCrude crystals were recrystallized from ethanol

출처 및 근거

ORD 기록
ord-3c162ac0662642e38fab20fffb0079d3
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727082

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