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

HRID 1510431노트

반응식

HRID 1510431 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-e4277477388d41c0b07a4ce80836a0d8
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211927B2

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