5-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]oct-3-ene → 5-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]octane

HRID 44455노트

반응식

HRID 44455 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]23[CH2:15][N:12]([CH2:13][CH2:14]2)[CH2:11][CH:10]=[CH:9]3)=[CH:4][N:3]=1>[Pt]=O.CO>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]23[CH2:15][N:12]([CH2:13][CH2:14]2)[CH2:11][CH2:10][CH2:9]3)=[CH:4][N:3]=1

참가 물질

4

반응물 1

HCID 102860575-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]oct-3-ene

생성물 1

HCID 862593785-(2-Bromopyrid-5-yl)-1-azabicyclo[3.2.1]octane수율 71.3%

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 887Methanol용매

실험 절차

1.95 g (7.354 mmol) of 5-(2-bromopyrid-5-yl)-1-azabicyclo[3.2.1]oct-3-ene (WO 03/057 697) are introduced into 40 ml of methanol in a hydrogenation flask, and 195 mg of platinum oxide are then placed in suspension. The medium is stirred at room temperature under a hydrogen pressure of 26 psi for 45 minutes. The reaction medium is filtered through diatomaceous earth and the solvent is removed by evaporation under reduced pressure. The residue obtained is purified by chromatography on a column of silica gel, eluting with a mixture of chloroform, methanol and aqueous ammonia in 95/5/0.5 proportions. 1.4 g of 5-(2-bromopyrid-5-yl)-1-azabicyclo[3.2.1]octane are obtained in the form of a waxy oil.

후처리

  1. filtrationThe reaction medium is filtered through diatomaceous earth
  2. customthe solvent is removed by evaporation under reduced pressure
  3. customThe residue obtained
  4. customis purified by chromatography on a column of silica gel
  5. washeluting with a mixture of chloroform, methanol and aqueous ammonia in 95/5/0.5 proportions

출처 및 근거

ORD 기록
ord-4c6c5a434ea042f290a8391d2cee8d12
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541440B2

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