Sodium Bicarbonate → N-(4-(4-(Ethyl(6-fluoro-6-methylheptyl)amino)-1-hydroxybutyl)phenyl)methanesulfonamide

HRID 1654303ノート

反応式

HRID 1654303 の反応式
[CH2:1]([NH:3][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].Br[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([F:29])([CH3:28])[CH3:27].C(=O)(O)[O-].[Na+]>C(#N)C>[CH2:1]([N:3]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([F:29])([CH3:28])[CH3:27])[CH2:4][CH2:5][CH2:6][CH:7]([C:9]1[CH:10]=[CH:11][C:12]([NH:15][S:16]([CH3:19])(=[O:17])=[O:18])=[CH:13][CH:14]=1)[OH:8])[CH3:2]

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 10750976Heptane, 1-bromo-6-fluoro-6-methyl-HCID 10779588N-(4-(4-(ethylamino)-1-hydroxybutyl)phenyl)methanesulfonamide

生成物 1

HCID 9823219N-(4-(4-(Ethyl(6-fluoro-6-methylheptyl)amino)-1-hydroxybutyl)phenyl)methanesulfonamide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

(Procedure B) A stirred mixture of the product from Example 7, Step II, (0.37 g, 0.00128 mol), the product from Step III above (0.298 g, 0.0141 mol), sodium bicarbonate (0.21 g, 0.0026 mol) and acetonitrile (11 ml) was refluxed for 5 hours and kept at ambient temperature for 18 hours. It was filtered and the solid was washed with acetonitrile. The filtrate was concentrated and the residue was chromatographed on silica gel with 10% MeOH--CH2Cl2 to give 0.332 g of the titled product, a compound of Formula I'. The mass spectrum had m/z 416 (M+).

後処理

  1. filtrationIt was filtered
  2. washthe solid was washed with acetonitrile
  3. concentrationThe filtrate was concentrated
  4. customthe residue was chromatographed on silica gel with 10% MeOH

出典と根拠

ORDレコード
ord-1fc28eef807a4c6295390210a500cfaa
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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