Phosphorus pentachloride → 4-Bromo-2-(methoxyimino)-3-oxobutanoyl chloride

HRID 990208노트

반응식

HRID 990208 반응식
[Br:1][CH2:2][C:3](=[O:11])[C:4](=[N:8][O:9][CH3:10])[C:5](O)=[O:6].P(Cl)(Cl)(Cl)(Cl)[Cl:13]>C(Cl)Cl>[Br:1][CH2:2][C:3](=[O:11])[C:4](=[N:8][O:9][CH3:10])[C:5]([Cl:13])=[O:6]

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 536512154-Bromo-2-(methoxyimino)-3-oxobutanoic acid

생성물 1

HCID 534266374-Bromo-2-(methoxyimino)-3-oxobutanoyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-20 °C

실험 절차

4-bromo-2-methoxyimino-3-oxobutyric acid (2.57 g) is added to methylene chloride (20 ml) and the solution is cooled to −20° C. Phosphorous pentachloride (2.5 g) is added in small lots over a period of 5 min while maintaining the temperature between −20° C. and −15° C. Thereafter, the temperature is slowly raised to −5° C. and the reaction mass is stirred at −5° C. to 0° C. until the starting material's absence is noted with TLC in about 30 mins. Aqueous workup was done to remove inorganic impurities and byproducts and the organic layer was dried over anhydrous sodium sulfate. This solution is taken as is for the next stage.

후처리

  1. temperaturewhile maintaining the temperature between −20° C. and −15° C
  2. temperatureThereafter, the temperature is slowly raised to −5° C.
  3. customto remove inorganic impurities and byproducts
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate

출처 및 근거

ORD 기록
ord-00dbb20c680f435888eaa5afdc29c8c4
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06458949B1

반응 노트

불러오는 중…