3-Methoxybenzylamine → HCID 57754052、化合物

HRID 226213

反応式

HRID 226213 の反応式
[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]([C@H:18]1[CH2:20][O:19]1)[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([F:17])[CH:11]=1)([CH3:4])([CH3:3])[CH3:2].[O-]S(C(F)(F)F)(=O)=O.[Li+].[CH3:31][O:32][C:33]1[CH:34]=[C:35]([CH:38]=[CH:39][CH:40]=1)[CH2:36][NH2:37].[Cl-].[NH4+]>C(#N)C>[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([F:17])[CH:11]=1)[C@H:18]([OH:19])[CH2:20][NH:37][CH2:36][C:35]1[CH:38]=[CH:39][CH:40]=[C:33]([O:32][CH3:31])[CH:34]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 211563-MethoxybenzylamineHCID 25517Ammonium ChlorideHCID 3664839Trifluoromethanesulfonic acid, lithium saltHCID 86616462(1R,2S)-[2-(3,4-difluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester

生成物 1

HCID 57754052HCID 57754052、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of (1R,2S)-[2-(3,4-difluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester (0.03 g, 0.1 mmol) in acetonitrile (1 mL) was treated with lithium triflate (0.032 g, 0.2 mmol) and stirred at ambient temperature for 20 minutes. Then 3-methoxybenzylamine (0.016 mL, 0.12 mmol) was added to the reaction neat in one portion. The reaction was stirred at ambient temperature for 14 hours. The reaction was poured into saturated ammonium chloride solution (5 mL), extracted with ethyl acetate, the organic phase separated, dried (MgSO4) and the solvent removed at reduced pressure. The product was obtained as an oil and used without further purification (0.041 g, 94%). MS: 437 (M+H, 100%).

後処理

  1. stirringThe reaction was stirred at ambient temperature for 14 hours
  2. extractionextracted with ethyl acetate
  3. customthe organic phase separated
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed at reduced pressure
  6. customThe product was obtained as an oil
  7. customused without further purification (0.041 g, 94%)

出典と根拠

ORDレコード
ord-102b0fd138274c048ebe5de232edecef
出典データセット
uspto-grants-2009_07
特許番号
US07557137B2

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