p-Toluenesulfonic acid → Ethyl 2,7-diazabicyclo[3.3.0]octane-2-carboxylate

HRID 1460752ノート

反応式

HRID 1460752 の反応式
[CH:1]12[CH2:8][N:7](C(OC(C)(C)C)=O)[CH2:6][CH:5]1[CH2:4][CH2:3][N:2]2[C:16]([O:18][CH2:19][CH3:20])=[O:17].C1(C)C=CC(S(O)(=O)=O)=CC=1>C(Cl)(Cl)Cl>[CH:1]12[CH2:8][NH:7][CH2:6][CH:5]1[CH2:4][CH2:3][N:2]2[C:16]([O:18][CH2:19][CH3:20])=[O:17]

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 191009335-(1,1-Dimethylethyl) 1-ethyl hexahydropyrrolo[3,4-b]pyrrole-1,5-dicarboxylate

生成物 1

HCID 15070028Ethyl 2,7-diazabicyclo[3.3.0]octane-2-carboxylate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

15.2 g (53.5 mmol) of 2-ethyl 7-tert.-butyl 2,7-diazabicyclo[3.3.0]octane-2,7-dicarboxylate in 100 ml of chloroform are heated under reflux for five hours with 10.5 g (55.3 mol) of para-toluenesulphonic acid. The mixture is washed with 50 ml of 10% strength sodium hydroxide solution, the organic phase is dried over potassium carbonate and concentrated, and the residue is distilled.

後処理

  1. washThe mixture is washed with 50 ml of 10% strength sodium hydroxide solution
  2. dry with materialthe organic phase is dried over potassium carbonate
  3. concentrationconcentrated
  4. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-d92ec5b94d0c4a09957258e16f8abbb2
出典データセット
uspto-grants-1991_12
特許番号
US05071999

反応ノート

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