Sulfuryl chloride → 4-Chloro-2-(n-propoxyimino)acetoacetic acid methyl ester

HRID 653296노트

반응식

HRID 653296 반응식
[CH3:1][O:2][C:3](=[O:13])[C:4](=[N:8][O:9][CH2:10][CH2:11][CH3:12])[C:5]([CH3:7])=[O:6].S(Cl)([Cl:17])(=O)=O>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:13])[C:4](=[N:8][O:9][CH2:10][CH2:11][CH3:12])[C:5]([CH2:7][Cl:17])=[O:6]

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 54207568HCID 54207568, 화합물

생성물 1

HCID 542547764-Chloro-2-(n-propoxyimino)acetoacetic acid methyl ester수율 94%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
40 °C

실험 절차

To a solution of 7.4 g of 2-(n-propoxyimino)acetoacetic acid methyl ester in 7.4 ml of acetic acid is added 5.5 g of sulfuryl chloride, and the mixture is stirred for 10 minutes at 40° C., then for 6 hours at room temperature. The reaction solution is poured into 100 ml of ice-water, and subjected to extraction twice with chloroform. The extract is washed with an aqueous solution of sodium chloride, and aqueous solution of sodium bicarbonate and water in this order, and dried over anhydrous sodium sulfate. The solvent is evaporated under reduced pressure to yield 8.2 g (94%) of 4-chloro-2-(n-propoxyimino)acetoacetic acid methyl ester as a pale yellow oily product.

후처리

  1. waitfor 6 hours at room temperature
  2. extractionsubjected to extraction twice with chloroform
  3. washThe extract is washed with an aqueous solution of sodium chloride, and aqueous solution of sodium bicarbonate and water in this order
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent is evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-ec75cdecea0f4c77bbd537747223f951
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04675397

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