Potassium Carbonate → Methyl-(3-methyl-butyl)-(5-nitro-pyridin-2-yl)-amine

HRID 2236204ノート

反応式

HRID 2236204 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[CH3:11][NH:12][CH2:13][CH2:14][CH:15]([CH3:17])[CH3:16].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.CCOC(C)=O>[CH3:11][N:12]([CH2:13][CH2:14][CH:15]([CH3:17])[CH3:16])[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 783082-Chloro-5-nitropyridineHCID 521020N,3-Dimethyl-1-butanamine

生成物 1

HCID 59301378Methyl-(3-methyl-butyl)-(5-nitro-pyridin-2-yl)-amine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2-Chloro-5-nitropyridine (158 mg, 1 mmol), N-methylisoamylamine (101 mg, 1 mmol), and finely ground potassium carbonate (419 mg, 3 mmol) were heated to 80° C. in 10 mL anhydrous DMF for 3.5 hrs. The mixture was diluted with EtOAc, extracted with H2O and dried over MgSO4. The EtOAc layer was filtered, evaporated to dryness to yield 220 mg. ES-MS calcd for C11H17N3O2 (m/e) 223.28, obsd 224.1 (M+H).

後処理

  1. extractionextracted with H2O
  2. dry with materialdried over MgSO4
  3. filtrationThe EtOAc layer was filtered
  4. customevaporated to dryness
  5. customto yield 220 mg

出典と根拠

ORDレコード
ord-6f61e8bc14c242cc840f6a3f99bd27f6
出典データセット
uspto-grants-2010_05
特許番号
US07714126B2

反応ノート

読み込み中…