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

HRID 352140

反応式

HRID 352140 の反応式
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]

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-170e38e4aac64852af941fe35fecce62
出典データセット
uspto-grants-2004_06
特許番号
US06743939B2

関連ノート

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