4-Methylmorpholine → 1,1-Dimethylethyl [4-(methoxymethylamino)-4-oxobutyl]-carbamate

HRID 352140

반응식

HRID 352140 반응식
Cl.CN[O:4][CH3:5].[CH3:6][N:7]1CCOCC1.Cl.CN(C)CCCN=C=NCC.[C:25]([O:29][C:30]([NH:32][CH2:33][CH2:34][CH2:35][C:36]([OH:38])=O)=[O:31])([CH3:28])([CH3:27])[CH3:26]>CN(C)C1C=CN=CC=1.ClCCl>[CH3:28][C:25]([O:29][C:30](=[O:31])[NH:32][CH2:33][CH2:34][CH2:35][C:36]([NH:7][CH2:6][O:4][CH3:5])=[O:38])([CH3:26])[CH3:27]

참가 물질

7

반응물 4

HCID 79724-MethylmorpholineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 2948944-(((Tert-butoxy)carbonyl)amino)butanoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 871517791,1-Dimethylethyl [4-(methoxymethylamino)-4-oxobutyl]-carbamate수율 83%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

4-(Dimethylamino)pyridine (6.11 g), N,O-dimethylhydroxylamine hydrochloride(4.88 g), N-methylmorpholine (5.06 g) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (9.58 g) were added in quick succession to a solution of 4-(tert-butoxycarbonylamino)butyric acid (10.16 g) in dichloromethane (200 ml). The reaction mixture was then stirred under ambient conditions for 18 h. The solution was then washed with 2M hydrochloric acid solution, 10% sodium bicarbonate solution and brine. The organic layer was separated, dried over magnesium sulfate, filtered and the filtrate evaporated to dryness to give the subtitle compound as a colourless oil (10.2 g, 83%).

후처리

  1. washThe solution was then washed with 2M hydrochloric acid solution, 10% sodium bicarbonate solution and brine
  2. customThe organic layer was separated
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customthe filtrate evaporated to dryness

출처 및 근거

ORD 기록
ord-170e38e4aac64852af941fe35fecce62
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743939B2

연결된 노트

불러오는 중…