Sodium Perchlorate → 6-Butylbenzo[b]quinolizinium perchlorate

HRID 742499노트

반응식

HRID 742499 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 190474766-Butylbenzo[b]quinolizinium perchlorate

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

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-).

후처리

  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

출처 및 근거

ORD 기록
ord-429027ca47fc4447926e26a45f658d29
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05554620

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