Flumexadol → HCID 118323819、化合物

HRID 1051388ノート

反応式

HRID 1051388 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([CH:9]2[O:14][CH2:13][CH2:12][NH:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.[F:17][C:18]([F:26])([F:25])[C:19](=[CH2:24])[C:20]([O:22][CH3:23])=[O:21]>>[F:17][C:18]([F:26])([F:25])[CH:19]([CH2:24][N:11]1[CH2:12][CH2:13][O:14][CH:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:15])[F:16])[CH:4]=2)[CH2:10]1)[C:20]([O:22][CH3:23])=[O:21]

参加物

3

反応物 2

HCID 65774FlumexadolHCID 2782391Methyl 2-(trifluoromethyl)acrylate

生成物 1

HCID 118323819HCID 118323819、化合物

実験手順

In a 5 mL round-bottomed flask, 2-(3-(trifluoromethyl)phenyl)morpholine (650 mg, 2.81 mmol) was combined with methyl 2-(trifluoromethyl)acrylate (650 mg, 4.22 mmol; added slowly) to give a colorless solution and stirred at room temperature for 50 min. The crude reaction mixture was concentrated in vacuo to give an oil. The crude material was purified by flash chromatography (silica gel, 40+S, 0% to 30% ethyl acetate in hexanes) to afford 850 mg (78%)(methyl 3,3,3-trifluoro-2-((2-(3-(trifluoromethyl)phenyl)morpholino)-methyl)propanoate as a clear liquid. MH+=386.

後処理

  1. additionadded slowly)
  2. customto give a colorless solution
  3. customThe crude reaction mixture
  4. concentrationwas concentrated in vacuo
  5. customto give an oil
  6. customThe crude material was purified by flash chromatography (silica gel, 40+S, 0% to 30% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-2bef9af9fcde4139945c44cbef9bcdcf
出典データセット
uspto-grants-2016_07
特許番号
US09388172B2

反応ノート

読み込み中…