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Methyl 3-methyl-5-(3-methylphenyl)-4-isoxazole carboxylate → 3-Methyl-5-(3-methylphenyl)-1,2-oxazole-4-carboxylic acid

HRID 1063351
ノート
印刷プレビュー

反応式

HRID 1063351 の反応式
[CH3:1][C:2]1[C:6]([C:7]([O:9]C)=[O:8])=[C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[CH:12]=2)[O:4][N:3]=1>O1CCCC1>[CH3:1][C:2]1[C:6]([C:7]([OH:9])=[O:8])=[C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[CH:12]=2)[O:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 22279613Methyl 3-methyl-5-(3-methylphenyl)-4-isoxazole carboxylate

生成物 1

HCID 222795143-Methyl-5-(3-methylphenyl)-1,2-oxazole-4-carboxylic acid収率 98.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 3-methyl-5-(3-methylphenyl)-4-isoxazole carboxylate (183 mg) was dissolved in tetrahydrofuran/distilled water=4/1 (2 ml). Lithium hydroxide (66.5 mg) was added at room temperature, and the mixture was stirred at that temperature for 20 hours. After the completion of the reaction, 5%-aqueous hydrochloric acid was added to acidify the system, and the reaction product was extracted by liquid separation using chloroform and washed with saturated aqueous solution of sodium chloride. The product was dried over sodium sulfate to concentrate and the residue was dried using a vacuum pump. Thus, a useful intermidiate, i.e., 3-methyl-5-(3-methylphenyl)-4-isoxazole carboxylic acid (169 mg, yield 98%) was obtained.

後処理

  1. distillationdistilled water=4/1 (2 ml)
  2. additionLithium hydroxide (66.5 mg) was added at room temperature
  3. customAfter the completion of the reaction, 5%-aqueous hydrochloric acid
  4. additionwas added
  5. extractionthe reaction product was extracted by liquid separation
  6. washwashed with saturated aqueous solution of sodium chloride
  7. dry with materialThe product was dried over sodium sulfate
  8. concentrationto concentrate
  9. customthe residue was dried

出典と根拠

ORDレコード
ord-cace0fdcf82842749459864c3f4ef8d8
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06964975B2

反応ノート

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