Benzene → 5-(1-Hydroxypropyl)-3-phenylisoxazole

HRID 1440316

反応式

HRID 1440316 の反応式
C1(C(NCl)=[O:8])C=CC=CC=1.[CH:11]#[C:12][CH:13]([OH:16])[CH2:14][CH3:15].C([N:19]([CH2:22][CH3:23])CC)C.[CH:24]1C=[CH:28][CH:27]=[CH:26][CH:25]=1>>[OH:16][CH:13]([C:14]1[O:8][N:19]=[C:22]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:15]=1)[CH2:12][CH3:11]

参加物

5

反応物 4

HCID 241BenzeneHCID 8471TriethylamineHCID 929811-Pentyn-3-olHCID 12256294Benzamide, N-chloro-

生成物 1

HCID 151807655-(1-Hydroxypropyl)-3-phenylisoxazole

実験手順

Dissolved in 200 ml of benzene were 18.5 g (0.12 mol) of benzenehydroxamic acid chloride synthesized in accordance with a known process [J.Org.Chem., 45, 3916 (1980)] and 10.0 g (0.12 mole) of 1-pentyne-3-ol, followed by the dropwise addition of 18 g (0.18 mol) of triethylamine under ice cooling. After they were reacted under reflux for 10 hours, the reaction mixture was washed with water and the organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. .The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby 5-(1-hydroxypropyl)-3-phenylisoxazole was obtained as colorless crystals.

後処理

  1. customAfter they were reacted
  2. temperatureunder reflux for 10 hours
  3. washthe reaction mixture was washed with water
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. custom.The resulting residue was purified by chromatography on a silica gel column (eluent: chloroform)

出典と根拠

ORDレコード
ord-d645da827fc04e31b200ba66e4e69009
出典データセット
uspto-grants-1996_03
特許番号
US05498619

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