Tetrahydrofuran → HCID 53886136、化合物

HRID 1004389ノート

反応式

HRID 1004389 の反応式
C1COCC1.Cl[C:7]1[C:12]([C:13]([F:16])([F:15])[F:14])=[CH:11][C:10]([Cl:17])=[CH:9][N:8]=1.[H-].[Na+].[CH3:20][O:21][N:22]=[C:23]([C:32]1[CH:36]=[C:35]([CH3:37])[O:34][N:33]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH2:30][OH:31]>O>[CH3:20][O:21][N:22]=[C:23]([C:32]1[CH:36]=[C:35]([CH3:37])[O:34][N:33]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH2:30][O:31][C:7]1[C:12]([C:13]([F:16])([F:15])[F:14])=[CH:11][C:10]([Cl:17])=[CH:9][N:8]=1

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 110421442,5-dichloro-3-(trifluoromethyl)pyridineHCID 542688772-hydroxymethylphenyl 5-methylisoxazol-3-yl ketone O-methyloxime

生成物 1

HCID 53886136HCID 53886136、化合物収率 96.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

THF (3 ml), 2,5-dichloro-3-trifluoromethylpyridine (0.32 g, 1.5 mmol) and 60% sodium hydride (0.05 g, 1.2 mmol) were added to 2-hydroxymethylphenyl 5-methylisoxazol-3-yl ketone O-methyloxime (0.25 g, 1.0 mmol) under ice-cooling, and the mixture was stirred at room temperature overnight. Water (100 ml) was added to the reaction mixture, and the mixture was extracted with ether (150 ml). The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to give 2-(5-chloro-3-trifluoromethyl-2-pyridyloxymethyl)phenyl 5-methylisoxazol-3-yl ketone O-methyloxime (0.41 g, yield: 96.3%) as colorless crystals.

後処理

  1. temperaturecooling
  2. extractionthe mixture was extracted with ether (150 ml)
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-084e8804a3da40ceab9d8c2f3b662f92
出典データセット
uspto-grants-2000_04
特許番号
US06048885

反応ノート

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