methyl[5-chloro-2-(4-ethyl-3-fluoropyridine-2-carbonyl)-1H-indol-3-yl]acetate → [5-Chloro-2-(4-ethyl-3-fluoropyridine-2-carbonyl)-1H-indol-3-yl]acetic Acid

HRID 396495ノート

反応式

HRID 396495 の反応式
C[O:2][C:3](=[O:26])[CH2:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:14])[CH:12]=2)[NH:7][C:6]=1[C:15]([C:17]1[C:22]([F:23])=[C:21]([CH2:24][CH3:25])[CH:20]=[CH:19][N:18]=1)=[O:16]>C(O)(=O)C.Cl>[Cl:14][C:11]1[CH:12]=[C:13]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6]([C:15]([C:17]1[C:22]([F:23])=[C:21]([CH2:24][CH3:25])[CH:20]=[CH:19][N:18]=1)=[O:16])=[C:5]2[CH2:4][C:3]([OH:26])=[O:2]

参加物

4

反応物 1

HCID 23003366methyl[5-chloro-2-(4-ethyl-3-fluoropyridine-2-carbonyl)-1H-indol-3-yl]acetate

生成物 1

HCID 18542322[5-Chloro-2-(4-ethyl-3-fluoropyridine-2-carbonyl)-1H-indol-3-yl]acetic Acid収率 93%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒

実験手順

A stirred solution of methyl[5-chloro-2-(4-ethyl-3-fluoropyridine-2-carbonyl)-1H-indol-3-yl]acetate (Example 111, 391.2 mg, 1.044 mmol) in acetic acid (12 ml) and 2N aqueous HCl (4 ml) was heated at reflux temperature for 24 h. After cooling to room temperature, the resulting mixture was concentrated. The residue was diluted in THF (100 ml), dried (MgSO4) and concentrated. The crude product was purified by recrystallization to afford 349.2 mg (93%) of the title compound.

後処理

  1. temperatureat reflux temperature for 24 h
  2. concentrationthe resulting mixture was concentrated
  3. additionThe residue was diluted in THF (100 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customThe crude product was purified by recrystallization

出典と根拠

ORDレコード
ord-489dbe877c0d4f6698843ec78e7566a7
出典データセット
uspto-grants-2003_08
特許番号
US06608070B1

反応ノート

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