Iodine → HCID 12786936、化合物

HRID 725690ノート

反応式

HRID 725690 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[N:5]=1)(=[O:3])[CH3:2].[I:11]I.C(O)(C)C.[N:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>>[I-:11].[Br:10][C:6]1[N:5]=[C:4]([C:1](=[O:3])[CH2:2][N+:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:9]=[CH:8][CH:7]=1

参加物

5

実験手順

To a stirred solution of 2-acetyl-6-bromopyridine (100 g; 0.5 mole) in 600 mL pyridine was added iodine (127 g; 0.5 mole). The mixture was heated on a steam bath for 45 minutes, and the product crystallized on cooling. The solid was filtered and the light yellow crystalline cake was rinsed twice with methylene chloride. After drying, 183 g (90%) was obtained. MP 176°-178° C.; silica gel TLC system: 95acetone: 5 isopropanol.

後処理

  1. temperatureThe mixture was heated on a steam bath for 45 minutes
  2. customthe product crystallized
  3. temperatureon cooling
  4. filtrationThe solid was filtered
  5. washthe light yellow crystalline cake was rinsed twice with methylene chloride
  6. customAfter drying
  7. custom183 g (90%) was obtained

出典と根拠

ORDレコード
ord-fdae55a513b742c28bcefa581f5a4824
出典データセット
uspto-grants-1998_01
特許番号
US05707603

反応ノート

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