Hydrochloric Acid → 3-[2-(4-Aminophenyl)ethyl]-4-hydroxybenzofuran

HRID 230908ノート

反応式

HRID 230908 の反応式
C([NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][C:13]2[C:17]3[C:18]([OH:22])=[CH:19][CH:20]=[CH:21][C:16]=3[O:15][CH:14]=2)=[CH:7][CH:6]=1)(=O)C.Cl.C(=O)([O-])O.[Na+]>C(O)CC>[NH2:4][C:5]1[CH:6]=[CH:7][C:8]([CH2:11][CH2:12][C:13]2[C:17]3[C:18]([OH:22])=[CH:19][CH:20]=[CH:21][C:16]=3[O:15][CH:14]=2)=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 671358873-[2-(4-Acetylaminophenyl)ethyl]-4-hydroxybenzofuran

生成物 1

HCID 671360293-[2-(4-Aminophenyl)ethyl]-4-hydroxybenzofuran収率 49.6%

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

A mixture of 3-[2-(4-acetylaminophenyl)ethyl]-4-hydroxybenzofuran (1.2 g) and n-propanol (4 mL)-5 mol/L aqueous sodium hydroxide solution (8 mL) was heated for ref lux overnight. The reaction mixture was cooled to room temperature. To the reaction mixture was added 2 mol/L hydrochloric acid (21 mL). The mixture was poured into a saturated aqueous sodium hydrogen carbonate solution, and the resulting mixture was extracted with ethylacetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was treated with ethyl acetate. The precipitated crystals were collected by filtration and dried under reduced pressure to give the title compound (0.51 g).

後処理

  1. temperaturewas heated for ref lux overnight
  2. extractionthe resulting mixture was extracted with ethylacetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. additionthe residue was treated with ethyl acetate
  7. filtrationThe precipitated crystals were collected by filtration
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-5bd16d54df774310a1d614d5cc883302
出典データセット
uspto-grants-2009_07
特許番号
US07566699B2

反応ノート

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