Ammonia → 114812-34-9

HRID 1463515ノート

反応式

HRID 1463515 の反応式
[CH2:1]([N:3]1[CH2:7][CH2:6][CH2:5][C@H:4]1[C:8]([O:10]CC)=O)[CH3:2].[NH3:13]>CO>[CH2:1]([N:3]1[CH2:7][CH2:6][CH2:5][C@H:4]1[C:8]([NH2:13])=[O:10])[CH3:2]

参加物

4

反応物 2

HCID 222AmmoniaHCID 10942897Ethyl (S)-(-)-1-Ethyl-2-pyrrolidinecarboxylate

生成物 1

HCID 10866443114812-34-9

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

Ethyl (-)-(S)-1-ethyl-2-pyrrolidinecarboxylate (3.4 g, 0.02 mol) was added to a cooled solution of MeOH (10 ml) and liquid NH3 (10 ml) in a stainless steel reaction bottle containing 3 g of 3 Å molecular sieves. The bottle was heated at 50° C. for 20 h. After cooling the solvent was allowed to evaporate. The product was dissolved in dry MeOH, filtered and the filtrate was evaporated under reduced pressure to give the title compound as white crystals in a quantitative yield (2.8 g). Recrystallization from n-hexane afforded 2.5 g (88%) of the amide, mp 107°-108° C. [α]D25 =-119° (c=0.5 MeOH). The enantiomeric purity was determined to 99.7% S-isomer.

後処理

  1. additioncontaining 3 g of 3 Å molecular sieves
  2. temperatureAfter cooling the solvent
  3. customto evaporate
  4. dissolutionThe product was dissolved in dry MeOH
  5. filtrationfiltered
  6. customthe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-7a8b6cc15a5d477fa91e0fe830a34132
出典データセット
uspto-grants-1994_04
特許番号
US05300660

反応ノート

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