反応 #312606

ord-881f6fc899104a928d52a0b649bc775f

反応方程式

O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl
triphosgene
COC1CCNCC1.Cl
4-methoxy-piperidine hydrochloride salt
c1ccncc1
pyridine
COC1CCN(C(=O)Cl)CC1
4-Methoxy-piperidine-1-carbonyl chloride

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過filtered through a silica pad
  2. 2
    洗浄eluting with dichloromethane
  3. 3
    その他evaporated
  4. 4
    その他After trituration with diisopropyl ether, the mixture was used without purification

実験手順

To a stirred solution of triphosgene (7.4 g, 0.025 mmol) in dichloromethane (200 ml) at ice bath was added dropwise a solution of 4-methoxy-piperidine hydrochloride salt (10 g, 0.066 mmol) and pyridine (10.9 g, 0.139 mmol) in dichloromethane (100 ml). The mixture was stirred over night and filtered through a silica pad, eluting with dichloromethane and evaporated. After trituration with diisopropyl ether, the mixture was used without purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07557101B2uspto-grants-2009_07