Hydrochloric Acid → 5-(4-Chlorophenyl)-4-methylisoxazole-3-carboxylic acid

HRID 1510431ノート

反応式

HRID 1510431 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:12][N:11]=[C:10]([C:13]([O:15]CC)=[O:14])[C:9]=2[CH3:18])=[CH:4][CH:3]=1.O.[OH-].[Li+].Cl>O1CCCC1.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[O:12][N:11]=[C:10]([C:13]([OH:15])=[O:14])[C:9]=2[CH3:18])=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 67121076Ethyl 5-(4-chlorophenyl)-4-methylisoxazole-3-carboxylate

生成物 1

HCID 671210815-(4-Chlorophenyl)-4-methylisoxazole-3-carboxylic acid収率 95.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl 5-(4-chlorophenyl)-4-methylisoxazole-3-carboxylate (63 mg, 0.24 mmol) in tetrahydrofuran (1.5 mL) was added a solution of lithium hydroxide hydrate (10 mg, 0.24 mmol) in water (1.5 mL). After stirring for 20 minutes, the reaction mixture was acidified with 1M HCl and extracted with dichloromethane three times. The combined dichloromethane extracts were washed with brine, dried over magnesium sulfate, and evaporated to obtain 5-(4-chlorophenyl)-4-methylisoxazole-3-carboxylic acid (55 mg, 0.23 mmol).

後処理

  1. extractionextracted with dichloromethane three times
  2. washThe combined dichloromethane extracts were washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-e4277477388d41c0b07a4ce80836a0d8
出典データセット
uspto-grants-2012_07
特許番号
US08211927B2

反応ノート

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