Water → HCID 70873408, 화합물

HRID 2172238노트

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HRID 2172238 반응식
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

참가 물질

6

반응물 4

HCID 962WaterHCID 62657Potassium Phosphate, TribasicHCID 13683259HCID 13683259, 화합물HCID 67275754HCID 67275754, 화합물

생성물 1

HCID 70873408HCID 70873408, 화합물수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-8c338f6e516347e18cbf405e765ab7b6
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051333B2

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