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 1687655ノート

反応式

HRID 1687655 の反応式
[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]

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-b545b81411d948b3b3c876b56e456cfd
出典データセット
uspto-grants-2012_04
特許番号
US08148391B2

反応ノート

読み込み中…