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

HRID 1654303노트

반응식

HRID 1654303 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

(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+).

후처리

  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

출처 및 근거

ORD 기록
ord-1fc28eef807a4c6295390210a500cfaa
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05405997

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