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Potassium Hydroxide → 5-(Chloromethyl)-1,2-oxazole-3-carboxylic acid

HRID 1952846
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HRID 1952846 반응식
[Cl:1][CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]([O:10]CC)=[O:9])[CH:4]=1.[OH-].[K+]>C(O)C>[Cl:1][CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]([OH:10])=[O:9])[CH:4]=1
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참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 14674306Ethyl 5-chloromethylisoxazole-3-carboxylate

생성물 1

HCID 218664495-(Chloromethyl)-1,2-oxazole-3-carboxylic acid수율 76.8%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
65 °C

실험 절차

47.3 g (250 mmol) of ethyl 5-chloromethylisoxazole-3-carboxylate in 150 ml of ethanol were mixed with 14 g (250 mmol) of potassium hydroxide, and the mixture was stirred at 60-70° C. for 6 h. After cooling and concentration under reduced pressure, the residue was taken up in water and extracted with ether, the aqueous phase was acidified with hydrochloric acid and then extracted several times with ether, and the ether phase was dried over sodium sulfate and concentrated under reduced pressure (oil pump, 50° C.). 31 g of the required product were obtained (77% of theory).

후처리

  1. temperatureAfter cooling
  2. concentrationconcentration under reduced pressure
  3. extractionextracted with ether
  4. extractionextracted several times with ether
  5. dry with materialthe ether phase was dried over sodium sulfate
  6. concentrationconcentrated under reduced pressure (oil pump, 50° C.)

출처 및 근거

ORD 기록
ord-f240dec859874514930a0cecc8b078e3
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06114358

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