Potassium Cyanide → 6-Butylbenzo[b]quinolizinium perchlorate

HRID 742491ノート

反応式

HRID 742491 の反応式
[C-]#N.[K+].[Br-].[CH:5]1[C:14]2[CH:13]=[C:12]3[CH:15]=[CH:16][CH:17]=[CH:18][C:11]3=[CH:10][N+:9]=2[CH:8]=[CH:7][CH:6]=1.[Cl:19]([O-:23])(=[O:22])(=[O:21])=[O:20].[Na+]>O.C(O)C.O>[Cl:19]([O-:23])(=[O:22])(=[O:21])=[O:20].[CH2:14]([C:10]1[N+:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:14]=2[CH:13]=[C:12]2[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=12)[CH2:5][CH2:6][CH3:7]

参加物

6

反応物 3

HCID 9032Potassium CyanideHCID 202130Benzo(b)quinolizinium, bromide (1:1)HCID 522606Sodium Perchlorate

生成物 1

HCID 190474766-Butylbenzo[b]quinolizinium perchlorate

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 19096565Water ethanol溶媒

実験手順

A solution of KCN (3g, 0.046 mol) in a minimum of water was added to a solution of benzo[b]quinolizinium bromide (10 g; 0.0385 mol) in 200 ml water. The resulting solid was extracted with an equal volume of methylene chloride. The above organic layer was heated and a solution of bromine (6.4 g) in methylene chloride was added. The resulting yellow solid was isolated, dissolved in ethanol/water, and the resulting solution was treated with sodium perchlorate solution. The perchlorate salt was filtered and recrystallized from ethanol to afford 2 g of 6-cyano-benzo[b]quinolizinium perchlorate (Formula II: R1 =R7 =H; R2 =CN; X- =ClO4-) as a solid.

後処理

  1. extractionThe resulting solid was extracted with an equal volume of methylene chloride
  2. temperatureThe above organic layer was heated
  3. additiona solution of bromine (6.4 g) in methylene chloride was added
  4. customThe resulting yellow solid was isolated
  5. filtrationThe perchlorate salt was filtered
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-efcb7a821f564bbbb580a1b07d16cc5b
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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