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

HRID 981071ノート

反応式

HRID 981071 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-ec84cea7a1794c7eb87ff7d58c2fb1a2
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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