Water → HCID 70873408、化合物

HRID 2172238ノート

反応式

HRID 2172238 の反応式
P([O-])([O-])([O-])=O.[K+].[K+].[K+].[CH2:9]([O:16][CH2:17][CH2:18][C:19]1([CH3:22])[CH2:21][O:20]1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[F:23][C:24]([F:48])([F:47])[O:25][C:26]1[CH:46]=[CH:45][C:29]([CH2:30][CH2:31][CH:32]2[CH2:37][CH2:36][N:35]([C:38]3[CH:43]=[CH:42][C:41]([OH:44])=[CH:40][CH:39]=3)[CH2:34][CH2:33]2)=[CH:28][CH:27]=1.O>C(O)C>[CH2:9]([O:16][CH2:17][CH2:18][C:19]([CH3:22])([OH:20])[CH2:21][O:44][C:41]1[CH:40]=[CH:39][C:38]([N:35]2[CH2:34][CH2:33][CH:32]([CH2:31][CH2:30][C:29]3[CH:28]=[CH:27][C:26]([O:25][C:24]([F:47])([F:23])[F:48])=[CH:46][CH:45]=3)[CH2:37][CH2:36]2)=[CH:43][CH:42]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 962WaterHCID 62657Potassium Phosphate, TribasicHCID 13683259HCID 13683259、化合物HCID 67275754HCID 67275754、化合物

生成物 1

HCID 70873408HCID 70873408、化合物収率 86%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A tripotassium phosphate (0.44 g, 2.1 mmol) was added to a solution of 2-[2-(Benzyloxy)ethyl]-2-methyloxirane (1.00 g, 5.2 mmol) and 4-{4-[4-(trifluoromethoxy)phenethyl]piperidin-1-yl}phenol (2.28 g, 6.2 mmol) in ethanol (10 ml), and then the mixture was heated at reflux overnight. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution, dried over sodium sulfate, and concentrated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0→50:50) to afford the title compound as a brown powder (2.43 g, 86%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux overnight
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe organic layer was washed with a saturated sodium chloride aqueous solution
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0→50:50)

出典と根拠

ORDレコード
ord-8c338f6e516347e18cbf405e765ab7b6
出典データセット
uspto-grants-2015_06
特許番号
US09051333B2

反応ノート

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