HCID 69004791、化合物 → HCID 69007001、化合物

HRID 2105550ノート

反応式

HRID 2105550 の反応式
C([O:5][C:6](=[O:29])[CH2:7][CH:8]1[C:14](=[O:15])[N:13](CC2C=CC(OC)=CC=2)[C:12]2[CH:25]=[CH:26][CH:27]=[CH:28][C:11]=2[CH2:10][CH2:9]1)(C)(C)C>C(O)(C(F)(F)F)=O>[O:15]=[C:14]1[NH:13][C:12]2[CH:25]=[CH:26][CH:27]=[CH:28][C:11]=2[CH2:10][CH2:9][CH:8]1[CH2:7][C:6]([OH:29])=[O:5]

参加物

3

反応物 1

HCID 69004791HCID 69004791、化合物

生成物 1

HCID 69007001HCID 69007001、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
100 °C

実験手順

[1-(4-Methoxy-benzyl)-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-3-yl]-acetic acid tert-butyl ester (0.19 mmol) is dissolved in 1.5 mL of TFA and heated to 100° C. for 3 hours. The mixture is cooled down to room temperature and concentrated. The residue is treated with NaOH (1N) (1 mL) and extracted with EtOAc (3×1 mL). The aqueous layer is then neutralized to pH=2 with HCl (1M) and extracted with EtOAc (3×2 mL). The organic layers resulted from this extraction is concentrated to provide the crude (2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-3-yl)-acetic acid. Yield: 72%.

後処理

  1. temperatureThe mixture is cooled down to room temperature
  2. concentrationconcentrated
  3. additionThe residue is treated with NaOH (1N) (1 mL)
  4. extractionextracted with EtOAc (3×1 mL)
  5. extractionextracted with EtOAc (3×2 mL)
  6. customThe organic layers resulted from this extraction
  7. concentrationis concentrated

出典と根拠

ORDレコード
ord-2cd9518aa3944d3fb277bd25a708793d
出典データセット
uspto-grants-2009_08
特許番号
US07579363B2

反応ノート

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