2-Methylaziridine → HCID 58070545, 화합물

HRID 563364

반응식

HRID 563364 반응식
[CH3:1][CH:2]1[CH2:4][NH:3]1.[OH-].[Na+].Cl[C:8]([CH2:10][CH2:11][O:12][C:13](=[O:16])[CH:14]=[CH2:15])=[O:9]>O.C(Cl)Cl>[CH3:1][CH:2]1[CH2:4][N:3]1[C:8](=[O:9])[CH2:10][CH2:11][O:12][C:13](=[O:16])[CH:14]=[CH2:15]

참가 물질

6

반응물 3

HCID 63772-MethylaziridineHCID 14798Sodium HydroxideHCID 57428991HCID 57428991, 화합물

생성물 1

HCID 58070545HCID 58070545, 화합물수율 74.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a stirred 0° C. solution of 2-methylaziridine (5.1 g, about 80 mmol, 90% pure, available from Aldrich) and NaOH (3.6 g, 90 mmol) in a mixture of 50 mL of water and 25 mL of methylene chloride was added dropwise a solution of acrylic acid-2-chlorocarbonylethyl ester (11.6 g, 59 mmol) in 25 mL of methylene chloride. When the addition was complete, the reaction flask was removed from the ice bath and the reaction mixture was allowed to warm to room temperature and was stirred overnight. The phases were then separated and the methylene chloride phase was washed once with 25 mL of water, dried over K2CO3, filtered, and solvent removed at reduced pressure to leave 8.1 g of acrylic acid-3-(2-methylaziridin-1yl)-3-oxopropyl ester as a colorless oil. NMR and IR spectral analyses confirmed the structure of the product.

후처리

  1. additionWhen the addition
  2. customthe reaction flask was removed from the ice bath
  3. customThe phases were then separated
  4. washthe methylene chloride phase was washed once with 25 mL of water
  5. dry with materialdried over K2CO3
  6. filtrationfiltered
  7. customsolvent removed at reduced pressure

출처 및 근거

ORD 기록
ord-dde0356272c34fa698deed97651dbf0b
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067504B2

연결된 노트

불러오는 중…