Sodium Hydroxide → 2,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester

HRID 1496685

반응식

HRID 1496685 반응식
[CH3:1][C:2]1[NH:3][C:4]([CH3:25])=[C:5]([C:21]([O:23]C)=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)[C:7]=1[C:8]([O:10][CH3:11])=[O:9].[OH-].[Na+]>CO>[CH3:11][O:10][C:8]([C:7]1[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)[C:5]([C:21]([OH:23])=[O:22])=[C:4]([CH3:25])[NH:3][C:2]=1[CH3:1])=[O:9]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 89082m-Nifedipine

생성물 1

HCID 1733222,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester수율 57.2%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

3.5 g dimethyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate (0.01 mol) and 150 mL methanol were mixed. To the mixture was added a saturated aqueous NaOH solution (9 g, 0.225 mol) under stirring. The reaction was conducted at 70° C. under violent stirring for 6 hours, and evaporated under reduced pressure to remove 80 mL methanol. To the residue was added 200 mL water. The unreacted starting materials are removed by filtration. The filtrate was adjusted to a pH of about 2.5 with 1 mol/L hydrochloric acid to separate a yellow solid, which was filtered and dried to produce a khaki powder. The resulting powder was treated with methanol to produce the title product as a yellow solid (1.9 g) in a yield of 57.2%.

후처리

  1. customwas conducted at 70° C.
  2. stirringunder violent stirring for 6 hours
  3. customevaporated under reduced pressure
  4. customto remove 80 mL methanol
  5. additionTo the residue was added 200 mL water
  6. customThe unreacted starting materials are removed by filtration
  7. customto separate a yellow solid, which
  8. filtrationwas filtered
  9. customdried
  10. customto produce a khaki powder

출처 및 근거

ORD 기록
ord-60c066ce929e440abb6a308e530d6fa5
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09198902B2

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