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

HRID 1085187

反応式

HRID 1085187 の反応式
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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回

実験手順

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: ##STR1514##

後処理

  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

出典と根拠

ORDレコード
ord-11a5e8bde42e4dcaac7dce7ca590c87a
出典データセット
uspto-grants-1991_04
特許番号
US05008257

関連ノート

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