Methanol → HCID 15232720、化合物

HRID 257617ノート

反応式

HRID 257617 の反応式
[C:1]1([C:7]2[N:8]=[C:9]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([OH:28])=[O:27])[O:10][C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:29]O>S(=O)(=O)(O)O.C(OCC)C>[C:1]1([C:7]2[N:8]=[C:9]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])[O:10][C:11]=2[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 2

HCID 887MethanolHCID 1319604,5-Diphenyl-2-oxazolenonanoic acid

生成物 1

HCID 15232720HCID 15232720、化合物収率 96%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 4,5-diphenyl-2-oxazole nonanoic acid (800 mg, 2 mmol), methanol (2 mL) and concentrated sulfuric acid (2 drops) was heated to reflux. After 2 hours, the solvent was evaporated and the residue partitioned between CH2Cl2 and water. The organic phase was separated, washed with saturated NaHCO3 solution, dried over sodium sulfate and concentrated in vacuo to leave an oil. Chromatography on a column of silica gel using a mixture of hexanes and diethyl ether (4:1) as eluent gave methyl 4,5-diphenyl-2-oxazolenonanoate (800 mg, 96%).

後処理

  1. temperaturewas heated to reflux
  2. customthe solvent was evaporated
  3. customthe residue partitioned between CH2Cl2 and water
  4. customThe organic phase was separated
  5. washwashed with saturated NaHCO3 solution
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. customto leave an oil

出典と根拠

ORDレコード
ord-78f90e43addb4234ade53f9ce9039d2e
出典データセット
uspto-grants-1993_11
特許番号
US05262540

反応ノート

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