Methanol → 1-Methyl-3-{N-[[beta-[3,4-bis(isobutyryloxy)phenyl]ethyl]]carbamoyl}-1,4-dihydropyridine

HRID 621690

반응식

HRID 621690 반응식
FC(F)(F)C([O-])=O.[CH3:8][N+:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15](=[O:37])[NH:16][CH2:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][C:26](=[O:30])[CH:27]([CH3:29])[CH3:28])=[C:21]([O:31][C:32](=[O:36])[CH:33]([CH3:35])[CH3:34])[CH:20]=2)[CH:10]=1.CO.C([O-])(O)=O.[Na+].S(S([O-])=O)([O-])=O.[Na+].[Na+]>O.CCOCC>[CH3:8][N:9]1[CH:14]=[CH:13][CH2:12][C:11]([C:15](=[O:37])[NH:16][CH2:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][C:26](=[O:30])[CH:27]([CH3:29])[CH3:28])=[C:21]([O:31][C:32](=[O:36])[CH:33]([CH3:35])[CH3:34])[CH:20]=2)=[CH:10]1

참가 물질

7

반응물 4

HCID 887MethanolHCID 24489Sodium DithioniteHCID 516892Sodium BicarbonateHCID 140504311-methyl-3-{N-[[beta-[3,4-bis(isobutyryloxy)phenyl]ethyl]]carbamoyl}-pyridinium trifluoroacetate

생성물 1

HCID 140504301-Methyl-3-{N-[[beta-[3,4-bis(isobutyryloxy)phenyl]ethyl]]carbamoyl}-1,4-dihydropyridine

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 0.55 g (1 mmol) of 1-methyl-3-{N-[[β-[3,4-bis(isobutyryloxy)phenyl]ethyl]]carbamoyl}pyridinium trifluoroacetate in 50 ml of deaerated water containing 10 ml of methanol was extracted three times with 30 ml portions of ether. To the resultant aqueous solution was added NaHCO3 (0.25 g, 3 mmol) and 50 ml of ethyl ether and the mixture was kept under nitrogen. To this ice-cold mixture was added sodium dithionite (0.52 g, 3 mmol) and the mixture was stirred vigorously for 30 minutes. The ether layer was separated and the aqueous layer was extracted twice with ether. The combined ether extracts were washed with water and dried over sodium sulfate. Ether was removed under vacuum, leaving an oily product. NMR analysis confirmed that the product has the structural formula: ##STR1577##

후처리

  1. customThe ether layer was separated
  2. extractionthe aqueous layer was extracted twice with ether
  3. washThe combined ether extracts were washed with water
  4. dry with materialdried over sodium sulfate
  5. customEther was removed under vacuum
  6. customleaving an oily product

출처 및 근거

ORD 기록
ord-d8467940aa214b2c85693fd7f87bb0b6
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824850

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