Methanol → 2-Methoxy-1-formylpiperidine

HRID 1995269노트

반응식

HRID 1995269 반응식
[CH:1]([N:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)=[O:2].[CH3:9][OH:10]>F[B-](F)(F)F.C[N+](C)(C)C.[Ni]>[CH:1]([N:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]1[O:10][CH3:9])=[O:2]

참가 물질

6

반응물 3

HCID 887MethanolHCID 174291-PiperidinecarboxaldehydeHCID 178435160HCID 178435160, 화합물

생성물 1

HCID 27236672-Methoxy-1-formylpiperidine수율 84.3%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 12621Tetramethylammonium tetrafluoroborate촉매

실험 절차

An electrode assembly consisting of an anode of glassy carbon, a nickel cathode and two bipolar connected electrodes of glassy carbon inserted between the two outer electrodes was fitted in the cell of the device as described in Example 1. All four electrodes were framed as described in Example 1. Polyethylene nets (mesh width 3×5 mm and thickness of filaments 0.5 mm) between the plates had the function of spacers. In this cell, a mixture of 4,800 g of 1-formylpiperidine, 13,600 g of methanol and 68 g of tetramethylammonium tetrafluoroborate was electrolyzed at 27.5 A, 45 volts and 25° C. for 27 hours and 33 minutes (corresponding to 2,273 Ahr). After distillative work up, 5,120 g of 1-formyl-2-methoxypiperidine were isolated, corresponding to a current efficiency of 80.3%.

후처리

  1. customwas fitted in the cell of the device
  2. custom45 volts and 25° C.
  3. customfor 27 hours
  4. custom33 minutes (corresponding to 2,273 Ahr)

출처 및 근거

ORD 기록
ord-6757a7b9055c41ae8896d4ecf776bc08
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04404082

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