反応 #2122488

ord-a4235c195d2e4a28a2782dc713e599bd

反応方程式

CON1CCC(O)CC1
1-Methoxy-piperidin-4-ol
CON1CCC(O)CC1
1-methoxy-piperidin-4-ol
CCN(CC)CC
triethylamine
CS(=O)(=O)Cl
Methanesulfonyl chloride
CON1CCC(OS(C)(=O)=O)CC1
methanesulfonic acid 1-methoxy-piperidin-4-yl ester
収率 126.3%

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITat room temperature for an additional 1 hour
  2. 2
    ろ過Then the mixture was filtered
  3. 3
    その他the solvent evaporated

実験手順

21 g 1-Methoxy-piperidin-4-ol (from Step 1) and 19.4 g triethylamine were dissolved in 200 ml ethyl acetate, and cooled to 0° C. 15.0 g Methanesulfonyl chloride was added slowly. The resulting white suspension was stirred at 0° C. for 1 hour, then at room temperature for an additional 1 hour. Then the mixture was filtered and the solvent evaporated, yielding 34.6 g of methanesulfonic acid 1-methoxy-piperidin-4-yl ester. This material was used for the next step without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08574607B2uspto-grants-2013_11