Methanol → Methyl 4-(2-aminophenyl)butanoate

HRID 448880

反応式

HRID 448880 の反応式
[NH:1]1[C:7](=[O:8])[CH2:6][CH2:5][CH2:4][C:3]2[CH:9]=[CH:10][CH:11]=[CH:12][C:2]1=2.[CH3:13][OH:14]>S(=O)(=O)(O)O>[CH3:13][O:14][C:7](=[O:8])[CH2:6][CH2:5][CH2:4][C:3]1[CH:9]=[CH:10][CH:11]=[CH:12][C:2]=1[NH2:1]

参加物

4

反応物 2

HCID 887MethanolHCID 2485801,3,4,5-Tetrahydro-2H-1-benzazepin-2-one

生成物 1

HCID 237256Methyl 4-(2-aminophenyl)butanoate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
70 °C

実験手順

To 1,3,4,5-tetrahydro-benzo[b]azepin-2-one (1 g, 6.2 mmol) in MeOH (8 mL), concentrated sulfuric acid (0.5 mL) was added and the mixture was stirred at room temperature for 2 hrs and at 70° C. for an additional hr. The solvent was removed and DCM and water were added. The organic layer was removed and the aqueous layer was basified with sat NaHCO3 and extracted with EtOAc (3×). The combined organic layers were washed with brine, dried (Na2SO4) and concentrated in vacuo to yield 4-(2-amino-phenyl)-butyric acid methyl ester (0.93 g). MS [M+H]+: 194.1; tR=1.49 min. (method 1)

後処理

  1. customThe solvent was removed
  2. additionDCM and water were added
  3. customThe organic layer was removed
  4. extractionextracted with EtOAc (3×)
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-acc10ee7f9b9480fb8ac2b7d8162df74
出典データセット
uspto-grants-2013_07
特許番号
US08481738B2

関連ノート

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