Sodium Hydroxide → HCID 117940033、化合物

HRID 2199845ノート

反応式

HRID 2199845 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][C:9]2=[O:12])=[CH:5][C:4]=1[N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1.CO.O.[F:22][C:23]([F:39])([F:38])[C:24]([C:30]1[CH:31]=[N:32][CH:33]=[C:34]([CH:37]=1)[CH:35]=O)([OH:29])[C:25]([F:28])([F:27])[F:26].[OH-].[Na+]>C(Cl)(Cl)Cl>[F:28][C:25]([F:26])([F:27])[C:24]([C:30]1[CH:37]=[C:34](/[CH:35]=[C:8]2/[C:9](=[O:12])[C:10]3[C:6]([CH2:7]/2)=[CH:5][C:4]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)=[C:3]([O:2][CH3:1])[CH:11]=3)[CH:33]=[N:32][CH:31]=1)([OH:29])[C:23]([F:39])([F:38])[F:22]

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 177581373-Pyridinecarboxaldehyde, 5-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]-HCID 22242641Methanol--water (1/1)HCID 1179401286-Methoxy-5-morpholino-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 117940033HCID 117940033、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 13 (0.1 g, 0.40 mmol)), MeOH/H2O (1:1), was added 5-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)nicotinaldehyde 259 (0.132 g, 0.485 mmol) and NaOH (0.032 g, 0.80 mmol). The reaction was stirred at RT for 6 h. The reaction mass was diluted with chloroform and washed with water (3×25 ml). The organic layer was dried over sodium sulphate and concentrated to get the crude 263, which was purified through flash chromatography by using 100-200 mesh silica gel. The compound was eluted at 30% ethyl acetate in hexane to afford yellow coloured solid (E)-2-((5-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)pyridin-3-yl)methylene)-6-methoxy-5-morpholino-2,3-dihydro-1H-inden-1-one 263.

後処理

  1. washwashed with water (3×25 ml)
  2. dry with materialThe organic layer was dried over sodium sulphate
  3. concentrationconcentrated
  4. customto get the crude 263, which
  5. customwas purified through flash chromatography
  6. washThe compound was eluted at 30% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-ee71da6821ef4eefaecb44e703d16d40
出典データセット
uspto-grants-2016_06
特許番号
US09359315B2

反応ノート

読み込み中…