Lithium Hydroxide → 3-Aminoisoxazole-5-carboxylic acid

HRID 1891410ノート

反応式

HRID 1891410 の反応式
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]([O:9]CC)=[O:8])[O:4][N:3]=1.[OH-].[Li+]>C(#N)C.O>[NH2:1][C:2]1[CH:6]=[C:5]([C:7]([OH:9])=[O:8])[O:4][N:3]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 11126498Ethyl 3-aminoisoxazole-5-carboxylate

生成物 1

HCID 552646873-Aminoisoxazole-5-carboxylic acid収率 90.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

To a solution of ethyl 3-aminoisoxazole-5-carboxylate (prepared according to Lepage, Francis; Hublot, Bernard; Adolphe, Pierre Sylvie. Preparation of alkyl 3-aminoisoxazole-5-carboxylates. Fr. Demande (1998), FR 2750425) (0.790 g, 5.06 mmol) in acetonitrile (28 mL) and water (9.5 mL) was added lithium hydroxide (0.550 g, 23.0 mmol). The resulting mixture was stirred at rt for 3 h. The reaction was quenched with 1 N HCl. Organic solvent was removed in vacuo. The resulting precipitate was filtered and dried to give the product as white solid (585 mg, 90%). LCMS calculated for C4H5N2O3 (M+H)+: m/z=129.0.

後処理

  1. customThe reaction was quenched with 1 N HCl
  2. customOrganic solvent was removed in vacuo
  3. filtrationThe resulting precipitate was filtered
  4. customdried

出典と根拠

ORDレコード
ord-906661068fda4ef5844c1bf1a44881ff
出典データセット
uspto-grants-2013_08
特許番号
US08507541B2

反応ノート

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