N,N-Dimethylglycine → 2-Dimethylamino-N-(5,5-dimethyl-8-nitro-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)-acetamide

HRID 1687655노트

반응식

HRID 1687655 반응식
[CH3:1][N:2]([CH2:4][C:5]([OH:7])=O)[CH3:3].CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.CN(C=O)C.[NH2:35][CH:36]1[CH2:42][C:41]([CH3:44])([CH3:43])[C:40]2[CH:45]=[CH:46][C:47]([N+:49]([O-:51])=[O:50])=[CH:48][C:39]=2[NH:38][C:37]1=[O:52]>CCOCC>[CH3:1][N:2]([CH3:3])[CH2:4][C:5]([NH:35][CH:36]1[CH2:42][C:41]([CH3:44])([CH3:43])[C:40]2[CH:45]=[CH:46][C:47]([N+:49]([O-:51])=[O:50])=[CH:48][C:39]=2[NH:38][C:37]1=[O:52])=[O:7]

참가 물질

7

반응물 5

HCID 673N,N-DimethylglycineHCID 6228DimethylformamideHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 672640283-amino-5,5-dimethyl-8-nitro-3,4-dihydro-1H-1-benzazepin-2-one

생성물 1

HCID 672640872-Dimethylamino-N-(5,5-dimethyl-8-nitro-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)-acetamide

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Dimethylamino-acetic acid (0.124 g, 1.20 mmol), EDCl (0.461 g, 2.41 mmol), HOBT (0.276 g, 2.05 mmol) and DMF (1.00 mL, 12.9 mmol) were stirred at rt for 30 minutes, followed by the addition of TEA (0.235 mL, 1.68 mmol) and 3-Amino-5,5-dimethyl-8-nitro-1,3,4,5-tetrahydro-1-benzazepin-2-one (0.300 g, 1.20 mmol). The reaction mixture was stirred at rt for 3 h, diluted with ether and washed with water. The organic layer was dried over MgSO4, filtered, and concentrated under reduced pressure. Title compound was isolated as a white solid (80 mg, 20%).

후처리

  1. washwashed with water
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b545b81411d948b3b3c876b56e456cfd
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148391B2

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