Sodium Perchlorate → 6-Butylbenzo[b]quinolizinium perchlorate

HRID 742499ノート

反応式

HRID 742499 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]([C:9]1[C:14]([CH2:15]O)=[CH:13][CH:12]=[CH:11][C:10]=1CO)O.[Cl:19]([O-:23])(=[O:22])(=[O:21])=[O:20].[Na+]>O=P(Cl)(Cl)Cl>[Cl:19]([O-:23])(=[O:22])(=[O:21])=[O:20].[CH2:7]([C:15]1[N+:1]2[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=2[CH:7]=[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=12)[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 2

HCID 522606Sodium PerchlorateHCID 117766291-(2-Pyridyl)-1-[2,6-di(hydroxymethyl)-phenyl]methanol

生成物 1

HCID 190474766-Butylbenzo[b]quinolizinium perchlorate

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

A mixture of 0.6 g (2.5 mmol) of 1-(2-pyridyl)-1-[2,6-di(hydroxymethyl)-phenyl]methanol and 10 ml of POCl3 was refluxed with stirring for 4 hours. The mixture was cooled, poured onto ice, stirred and treated with a 20% sodium perchlorate solution. The resulting mixture was filtered, the resulting solid was washed with water, and dried to afford 0.58 g of 10-chloromethylrbenzo[b]quinolizinium perchlorate (Formula II: R1 =R2 =H; R7 =10--CH2Cl; X- =ClO4-).

後処理

  1. temperaturewas refluxed
  2. temperatureThe mixture was cooled
  3. additionpoured onto ice
  4. stirringstirred
  5. filtrationThe resulting mixture was filtered
  6. washthe resulting solid was washed with water
  7. customdried

出典と根拠

ORDレコード
ord-429027ca47fc4447926e26a45f658d29
出典データセット
uspto-grants-1996_09
特許番号
US05554620

反応ノート

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