Ammonia → 1-Azabicyclo[3.1.1]heptane-5-carboxamide

HRID 466812노트

반응식

HRID 466812 반응식
[N:1]12[CH2:7][C:5]([C:8]([O:10]C)=O)([CH2:6]1)[CH2:4][CH2:3][CH2:2]2.[NH3:12].C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl>[N:1]12[CH2:7][C:5]([C:8]([NH2:12])=[O:10])([CH2:6]1)[CH2:4][CH2:3][CH2:2]2

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 11430Potassium CarbonateHCID 19814748Methyl 1-azabicyclo[3.1.1]hept-5-ylcarboxylate

생성물 1

HCID 198147681-Azabicyclo[3.1.1]heptane-5-carboxamide

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Methyl 1-azabicyclo[3.1.1]hept-5-ylcarboxylate (D4, 1.35 g, 0.0087 mole) was treated with 20M aqueous ammonia solution (25 ml) and the mixture stirred at room temperature for 2 days. The solution was saturated with potassium carbonate and shaken with chloroform (40 ml) The mixture separated into three layers. The chloroform solution contained some product, however the majority was in the middle layer. These two were combined and concentrated in vacuo and the residue then treated with toluene (60 ml) and again concentrated in vacuo to azeotrope out the water. The title compound (D12) remained as a white solid (1.07 g, 88%) m.p. 188°-1920° C.

후처리

  1. customseparated into three layers
  2. concentrationconcentrated in vacuo
  3. additionthe residue then treated with toluene (60 ml)
  4. concentrationagain concentrated in vacuo

출처 및 근거

ORD 기록
ord-c2d116e29ed4478dadb10cba8e5b15ae
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05157160

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