Water → 1,1-Dimethylethyl N-[2-[(2,2,2-trifluoroethyl)amino]ethyl]carbamate

HRID 1893504노트

반응식

HRID 1893504 반응식
[F:1][C:2]([F:17])([F:16])[C:3]([NH:5][CH2:6][CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[F:1][C:2]([F:16])([F:17])[CH2:3][NH:5][CH2:6][CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:12])([CH3:14])[CH3:13]

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 15814419tert-Butyl [2-[(trifluoroacetyl)amino]ethyl]carbamateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 866507731,1-Dimethylethyl N-[2-[(2,2,2-trifluoroethyl)amino]ethyl]carbamate수율 74%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The compound (6.57 g, 25.6 mmol) obtained in step A was dissolved in tetrahydrofuran (100 ml), and the mixture was stirred under ice-cooling. Then, a suspension of lithium aluminum hydride (1.94 g, 51.2 mmol) in tetrahydrofuran (50 ml) was slowly added dropwise. Thereafter, the mixture was stood overnight at room temperature. The reaction mixture was ice-cooled again, water (2 ml), 1N aqueous sodium hydroxide solution (4 ml) and water (2 ml) were added in this order with stirring, and the mixture was stirred at room temperature for 5 hr. The insoluble material was filtered off through celite, and the obtained solution was concentrated under reduced pressure to give the title compound (4.56 g, yield 74%) as a yellow oil.

후처리

  1. temperaturecooling
  2. additionwas slowly added dropwise
  3. temperaturecooled again
  4. stirringwith stirring
  5. stirringthe mixture was stirred at room temperature for 5 hr
  6. filtrationThe insoluble material was filtered off through celite
  7. concentrationthe obtained solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7d78a15203cd4cacbf493dbd66b08aa3
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513235B2

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