Sodium Bicarbonate → Dimethyl 2-methyl-4-(2-nitrophenyl)-6-formyl-1,4-dihydropyridine-3,5-dicarboxylate

HRID 1248730노트

반응식

HRID 1248730 반응식
[CH3:1][C:2]1[NH:3][C:4]([CH:25](OC)[O:26]C)=[C:5]([C:21]([O:23][CH3:24])=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[N+:18]([O-:20])=[O:19])[C:7]=1[C:8]([O:10][CH3:11])=[O:9].C(=O)(O)[O-].[Na+]>CC(C)=O.Cl>[CH3:1][C:2]1[NH:3][C:4]([CH:25]=[O:26])=[C:5]([C:21]([O:23][CH3:24])=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[N+:18]([O-:20])=[O:19])[C:7]=1[C:8]([O:10][CH3:11])=[O:9]

참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 12896948HCID 12896948, 화합물

생성물 1

HCID 15737325Dimethyl 2-methyl-4-(2-nitrophenyl)-6-formyl-1,4-dihydropyridine-3,5-dicarboxylate수율 98.5%

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 313Hydrochloric Acid용매

반응 조건

온도
25 °C

실험 절차

A mixture of a solution of dimethyl 2-methyl-4-(2-nitrophenyl)-6-dimethoxymethyl-1,4-dihydropyridine-3,5-dicarboxylate (10.68 g) in acetone (110 ml) and 6N hydrochloric acid (10 ml) was stirred at 25° C. for 3 hours, which was neutralized with an aqueous sodium bicarbonate solution and acetone was distilled off under reduced pressure. The resultant reddish yellow oily precipitates were solidified, which were cracked finely, collected by filtration, washed with water and air dried over-night to give crude crystals of dimethyl 2-methyl-4-(2-nitrophenyl)-6-formyl-1,4-dihydropyridine-3,5-dicarboxylate (9.33 g).

후처리

  1. distillationwas distilled off under reduced pressure
  2. customThe resultant reddish yellow oily precipitates
  3. filtrationcollected by filtration
  4. washwashed with water and air
  5. customdried over-night

출처 및 근거

ORD 기록
ord-973325ed84964349b0bab3c29f36d74b
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04525478

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