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

HRID 981111ノート

反応式

HRID 981111 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1e235ef8731b471792c2172ae06fe340
出典データセット
uspto-grants-1991_02
特許番号
US04990517

反応ノート

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