Water → HCID 33240185, 화합물

HRID 1027478노트

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HRID 1027478 반응식
C(N(CC)CC)C.Cl.[CH2:9]([O:11][C:12](=[O:20])[CH:13]([NH2:19])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH3:10].[F:21][C:22]1[CH:23]=[C:24]([CH:28]=[CH:29][CH:30]=1)[C:25](Cl)=[O:26].O>ClCCl>[CH2:17]([O:16][C:14](=[O:15])[CH:13]([NH:19][C:25](=[O:26])[C:24]1[CH:28]=[CH:29][CH:30]=[C:22]([F:21])[CH:23]=1)[C:12]([O:11][CH2:9][CH3:10])=[O:20])[CH3:18]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 743763-Fluorobenzoyl chlorideHCID 3084143Propanedioic acid, 2-amino-, 1,3-diethyl ester, hydrochloride (1:1)

생성물 1

HCID 33240185HCID 33240185, 화합물수율 94.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

36.1 ml of triethylamine were added to a solution of 25 g of aminomalonic acid diethyl ester hydrochloride in 200 ml of dichloromethane with cooling in an ice bath. Then a solution of 18.7 g of 3-fluoro-benzoyl chloride in 100 ml of dichloromethane was added dropwise. After stirring for 2 h at 0° C., 100 ml of water were added dropwise. The layers were separated, and the aqueous layer was extracted with 100 ml of dichloromethane. The combined organic layers were dried with magnesium sulfate, filtered and evaporated to give 33.2 g of the crude title compound.

후처리

  1. temperaturewith cooling in an ice bath
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with 100 ml of dichloromethane
  4. dry with materialThe combined organic layers were dried with magnesium sulfate
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-ebf9bae0f01946c8878fe652c69c9b5e
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08735387B2

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