Methanol → HCID 43147868、化合物

HRID 1258800ノート

反応式

HRID 1258800 の反応式
O=S(Cl)Cl.[NH2:5][CH:6]([C:11]1[S:12][CH:13]=[CH:14][C:15]=1[CH3:16])[CH2:7][C:8]([OH:10])=[O:9].[CH3:17]O>>[NH2:5][CH:6]([C:11]1[S:12][CH:13]=[CH:14][C:15]=1[CH3:16])[CH2:7][C:8]([O:10][CH3:17])=[O:9]

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 247011743-Amino-3-(3-methylthiophen-2-yl)propanoic acid

生成物 1

HCID 43147868HCID 43147868、化合物

実験手順

To a 50 mL round bottom flask equipped with an electromagnetic stirrer and a drying tube, 15 mL of anhydrous methanol was added. The solution was cooled in an ice water-sodium chloride bath to minus 10° C., and 2 mL of SOCl2 was added slowly. The reaction mixture was allowed to react for an hour at room temperature. Then 1.85 g of 3-amino-3-(3-methyl-thiophene-2-yl)propionic acid was added. The mixture was allowed to react for 3 hours at room temperature, then refluxed for 40 minutes. After the solution was evaporated to remove the solvent, 100 mL of CHCl3 and 100 mL saturated NaHCO3 were added, and the layers were separated. The organic layer was washed successively with 30 mL of water and 30 mL of saturated brine, dried over anhydrous MgSO4, filtered, evaporated, and purified by column chromatography to give an oil-like product. MS (m/z): 200 [M+1]+.

後処理

  1. customTo a 50 mL round bottom flask equipped with an electromagnetic stirrer and a drying tube
  2. additionwas added slowly
  3. customto react for an hour at room temperature
  4. customto react for 3 hours at room temperature
  5. temperaturerefluxed for 40 minutes
  6. customAfter the solution was evaporated
  7. customto remove the solvent, 100 mL of CHCl3 and 100 mL saturated NaHCO3
  8. additionwere added
  9. customthe layers were separated
  10. washThe organic layer was washed successively with 30 mL of water and 30 mL of saturated brine
  11. dry with materialdried over anhydrous MgSO4
  12. filtrationfiltered
  13. customevaporated
  14. custompurified by column chromatography
  15. customto give an oil-like product

出典と根拠

ORDレコード
ord-1f77988209dd461db17d03cc33b9644c
出典データセット
uspto-grants-2013_06
特許番号
US08466191B2

反応ノート

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