Potassium Carbonate → N-(4-(4-(Ethyl(6-hydroxy-6-methylheptyl)amino)-1-hydroxybutyl)phenyl)methanesulfonamide

HRID 1654299ノート

反応式

HRID 1654299 の反応式
[CH2:1]([N:3]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][C:25]([O:28]C(=O)C)([CH3:27])[CH3:26])[CH2:4][CH2:5][CH2:6][CH:7]([C:9]1[CH:14]=[CH:13][C:12]([NH:15][S:16]([CH3:19])(=[O:18])=[O:17])=[CH:11][CH:10]=1)[OH:8])[CH3:2].C([O-])([O-])=O.[K+].[K+]>CO.O>[CH2:1]([N:3]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][C:25]([OH:28])([CH3:27])[CH3:26])[CH2:4][CH2:5][CH2:6][CH:7]([C:9]1[CH:14]=[CH:13][C:12]([NH:15][S:16]([CH3:19])(=[O:17])=[O:18])=[CH:11][CH:10]=1)[OH:8])[CH3:2]

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 15294456N-(4-(4-(Ethyl(6-acetoxy-6-methylheptyl)amino)-1-hydroxybutyl)phenyl)methanesulfonamide

生成物 1

HCID 15294457N-(4-(4-(Ethyl(6-hydroxy-6-methylheptyl)amino)-1-hydroxybutyl)phenyl)methanesulfonamide収率 89.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A stirred solution of the product from Example 13 (1.35 g, 0.00296 mol) in methanol (80 ml) was treated with a solution of K2CO3 (2.04 g, 0.0148 mol) in water (5.9 ml) and the mixture was refluxed for 21.5 hours. It was kept at ambient temperature for 42.5 hours and concentrated to an aqueous residue which was mixed with water (10 ml) and CH2Cl2, acidified to pH 8.5-9 with 6 NHCl, saturated with NaCl and extracted with CH2Cl2. The extract was dried (MgSO4), concentrated and the residue chromatographed on silica gel with 0.5% NH4OH-9% MeOH--CH2Cl2 to give 1.1 g of the titled compound which is a compound of Formula I'. The high resolution mass spectrum had m/z 414(M+). Theory for C21H38N2O4S: 414.2552; measured: 414.2560.

後処理

  1. temperaturethe mixture was refluxed for 21.5 hours
  2. concentrationconcentrated to an aqueous residue which
  3. additionwas mixed with water (10 ml) and CH2Cl2
  4. extractionextracted with CH2Cl2
  5. dry with materialThe extract was dried (MgSO4)
  6. concentrationconcentrated
  7. customthe residue chromatographed on silica gel with 0.5% NH4OH-9% MeOH

出典と根拠

ORDレコード
ord-4103e2810d4c4e10bf150b4c59b1a6e2
出典データセット
uspto-grants-1995_04
特許番号
US05405997

反応ノート

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