Dimethylamine → 2-(N,N-Dimethylamino)-6-Iodopyrazine

HRID 256884

反応式

HRID 256884 の反応式
I[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([I:8])[N:3]=1.[CH3:9][NH:10][CH3:11]>CO>[I:8][C:4]1[CH:5]=[N:6][CH:7]=[C:2]([N:10]([CH3:11])[CH3:9])[N:3]=1

参加物

4

反応物 2

HCID 674DimethylamineHCID 110020782,6-Diiodopyrazine

生成物 1

HCID 157501312-(N,N-Dimethylamino)-6-Iodopyrazine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2,6-diiodopyrazine (6 g, 18.1 mmol) in methanol (50 ml) and dimethylamine (40% aqueous solution, 200 ml) was heated at reflux for 1 h. The methanol was removed under vacuum, the aqueous saturated with potassium carbonate and extracted with dichloromethane (3×100 ml). The combined extracts were dried (Na2SO4), evaporated and the residue purified by chromatography through silica-gel eluting with dichloromethane. The product (4 g) was obtained as a low melting solid, m.p. 46°-48° C., m/e 249 (M+); δ (360 MHz, CDCl3) 3.10 (6H, s, 2×Me); 7.87 (1H, s, pyrazine-H); 8.01 (1H, s, pyrazine-H).

後処理

  1. temperatureat reflux for 1 h
  2. customThe methanol was removed under vacuum
  3. extractionthe aqueous saturated with potassium carbonate and extracted with dichloromethane (3×100 ml)
  4. dry with materialThe combined extracts were dried (Na2SO4)
  5. customevaporated
  6. customthe residue purified by chromatography through silica-gel
  7. washeluting with dichloromethane

出典と根拠

ORDレコード
ord-5e6592da0d65436e8bf54cdc85ddec51
出典データセット
uspto-grants-1993_11
特許番号
US05260293

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