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

HRID 981071노트

반응식

HRID 981071 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ec84cea7a1794c7eb87ff7d58c2fb1a2
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04990517

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