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N,N-Dimethylglycine → 2-Dimethylamino-N-(5-methyl-6-oxo-5,6-dihydro-phenanthridin-8-yl)-acetamide

HRID 968290
ノート
印刷プレビュー

反応式

HRID 968290 の反応式
Cl.CN(C)CCCN=C=NCC.[NH2:13][C:14]1[CH:15]=[C:16]2[C:25](=[CH:26][CH:27]=1)[C:24]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[N:18]([CH2:28]C)[C:17]2=[O:30].[CH3:31][N:32]([CH3:37])[CH2:33][C:34](O)=[O:35].C(N(CC)CC)C>ClCCl>[CH3:31][N:32]([CH3:37])[CH2:33][C:34]([NH:13][C:14]1[CH:15]=[C:16]2[C:25](=[CH:26][CH:27]=1)[C:24]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[N:18]([CH3:28])[C:17]2=[O:30])=[O:35]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 673N,N-DimethylglycineHCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 222885418-amino-5-ethyl-5H-phenanthridin-6-one

生成物 1

HCID 222885432-Dimethylamino-N-(5-methyl-6-oxo-5,6-dihydro-phenanthridin-8-yl)-acetamide収率 33.5%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

1-[3-(Dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (EDC) (63 mg, 0.33 mmol) was added in one portion to a solution of 8-amino-5-ethyl-5H-phenanthridin-6-one I-16c (65 mg, 0.27 mmol), N,N-dimethylglycine (34 mg, 0.33 mmol) 4-dimethylaminopyridine (7 mg, 0.054 mmol), and triethylamine (0.076 ml, 0.55 mmol) in dichloromethane (5 ml). The resultant solution was stirred at 23° C. for 16 hours and diluted with 1:1 ethyl acetate/hexanes (20 ml). The reaction mixture was washed with water (25 ml) and saturated aqueous ammonium chloride (25 ml) and dried over anhydrous magnesium sulfate and concentrated. The residue was purified by rotary chromatography on silica gel (dichloromethane grading to 5% methanol/dichloromethane) to provide 2-dimethylamino-N-(5-methyl-6-oxo-5,6-di hydro-phenanthridin-8-yl)-acetamide 16A (28 mg, 33%) as a yellow oil.

後処理

  1. washThe reaction mixture was washed with water (25 ml) and saturated aqueous ammonium chloride (25 ml)
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by rotary chromatography on silica gel (dichloromethane grading to 5% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-6f04bccc9ed547e386572b052de4c88a
出典データセット
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06958347B2

反応ノート

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