Acetic Acid → trans-1-Benzyl-3-hydroxy-4-methoxypyrrolidine

HRID 345781ノート

反応式

HRID 345781 の反応式
[CH2:1]([N:8]1CC2[CH:10]([O:11]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:14][O-].[Na+].[C:17]([OH:20])(=O)[CH3:18]>CO>[CH2:1]([N:8]1[CH2:18][C@@H:17]([O:20][CH3:14])[C@H:10]([OH:11])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 98153703-Benzyl-6-oxa-3-azabicyclo(3.1.0)hexaneHCID 10942334Sodium Methoxide

生成物 1

HCID 15069965trans-1-Benzyl-3-hydroxy-4-methoxypyrrolidine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

34.9 g (0.2 mol) of 3-benzyl-6-oxa-3-azabicyclo[3.1.0]hexane (U.S. Pat. No. 4,254,135) are heated with 3.6 g (20 mmol) of sodium methylate solution (30% strength) at 120° C. in 200 ml of absolute methanol in an autoclave for 10 hours. After cooling, the mixture is neutralized with 1.2 g (20 mmol) of acetic acid and the solvent is removed on a rotary evaporator. The residue is taken up in tetrahydrofuran and the sodium acetate is filtered off. The filtrate is concentrated and the residue is distilled.

後処理

  1. temperatureAfter cooling
  2. customthe solvent is removed on a rotary evaporator
  3. filtrationthe sodium acetate is filtered off
  4. concentrationThe filtrate is concentrated
  5. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-b601ff63d30340c78c0b43792f50c68b
出典データセット
uspto-grants-1991_10
特許番号
US05059597

反応ノート

読み込み中…