Perchloric Acid → Ethyl 3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

HRID 36691노트

반응식

HRID 36691 반응식
O1CCCCC1[N:7]1[O:14][CH2:13][CH:12]2[CH:8]1[CH2:9][N:10]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11]2.Cl(O)(=O)(=O)=O.C[O-].[Na+]>C(O)C>[CH:8]12[CH2:9][N:10]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:11][CH:12]1[CH2:13][O:14][NH:7]2

참가 물질

5

반응물 3

HCID 24247Perchloric AcidHCID 10942334Sodium MethoxideHCID 15070014Ethyl 2-(tetrahydropyran-2-yl)-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

생성물 1

HCID 15070015Ethyl 3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

15 g (55.5 mmol) of ethyl 2-(tetrahydropyran-2-yl)-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 8.25 g (56 mmol) of 70% strength perchloric acid in 100 ml of ethanol for 30 minutes. 10.5 g (58 mmol) of 30 strength sodium methylate solution are added, the mixture is concentrated, the residue is taken up in water and the solution is saturated with K2CO3 and extracted with CHCl3. The extract is dried over K2CO3 and concentrated and the residue is distilled.

후처리

  1. concentrationthe mixture is concentrated
  2. extractionextracted with CHCl3
  3. dry with materialThe extract is dried over K2CO3
  4. concentrationconcentrated
  5. distillationthe residue is distilled

출처 및 근거

ORD 기록
ord-6304a62e9af14528a5461e06a6e88092
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416096

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