Trimethylphosphine → (E)-ethyl 3-(4-(4-(N-(2-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)ethyl)sulfamoyl)phenoxy)-3,5-difluorophenyl)-2-methylacrylate

HRID 45692

反応式

HRID 45692 の反応式
[N:1]([CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][NH:15][S:16]([C:19]1[CH:41]=[CH:40][C:22]([O:23][C:24]2[C:29]([F:30])=[CH:28][C:27](/[CH:31]=[C:32](\[CH3:38])/[C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:26][C:25]=2[F:39])=[CH:21][CH:20]=1)(=[O:18])=[O:17])=[N+]=[N-].CP(C)C>C1COCC1.O>[NH2:1][CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][NH:15][S:16]([C:19]1[CH:41]=[CH:40][C:22]([O:23][C:24]2[C:25]([F:39])=[CH:26][C:27](/[CH:31]=[C:32](\[CH3:38])/[C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:28][C:29]=2[F:30])=[CH:21][CH:20]=1)(=[O:18])=[O:17]

参加物

5

実験手順

To a solution of (E)-ethyl 3-(4-(4-(N-(2-(2-(2-(2-azidoethoxy)ethoxy)ethoxy)ethyl)sulfamoyl)phenoxy)-3,5-difluorophenyl)-2-methylacrylate (169 mg, 0.28 mmol) in THF (6 ml) and water (0.6 mL) under nitrogen was added trimethylphosphine (26 mg, 0.34 mmol). After stirring for 3 hours, the solvents were removed at reduced pressure and. The residue was dissolved in water (5 mL) and extracted with EtOAc (3×25 mL). The combined organic layers were dried (Na2SO4) and concentrated to give the title compound (162 mg).

後処理

  1. customthe solvents were removed at reduced pressure
  2. dissolutionThe residue was dissolved in water (5 mL)
  3. extractionextracted with EtOAc (3×25 mL)
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-f0f35b582d2a47409c67cb13c6948bc4
出典データセット
uspto-grants-2013_09
特許番号
US08541448B2

関連ノート

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