Ammonia → 114812-34-9

HRID 1463515노트

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HRID 1463515 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 10866443114812-34-9

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7a8b6cc15a5d477fa91e0fe830a34132
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05300660

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