Potassium Cyanide → 6-Butylbenzo[b]quinolizinium perchlorate

HRID 742491노트

반응식

HRID 742491 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 190474766-Butylbenzo[b]quinolizinium perchlorate

시약·촉매·용매 2

HCID 962Water용매2회HCID 19096565Water ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-efcb7a821f564bbbb580a1b07d16cc5b
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05554620

반응 노트

불러오는 중…