Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) → HCID 54228902, 화합물

HRID 75120노트

반응식

HRID 75120 반응식
[O:1]1[CH:7]=[CH:6][CH:5]=[N:4][C:3](=[O:8])[CH2:2]1.F[B-](F)(F)F.[CH3:14][O+](C)C>C(Cl)Cl>[CH3:14][O:8][C:3]1[CH2:2][O:1][CH2:7][CH2:6][CH2:5][N:4]=1

참가 물질

4

반응물 2

HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 536461591,4-Oxazepine-3-one

생성물 1

HCID 54228902HCID 54228902, 화합물수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The product from step 4 (1.06 g, 9.2 mmol) was dissolved in 11 mL of DCM and the stirred solution was treated with trimethyloxonium tetrafluoroborate (1.70 g, 11.5 mmol) and the mixture was stirred for 4 hours. The reaction was quenched by addition of 1.70 mL saturated aqueous K2CO3 and the mixture was vigorously stirred for 15 minutes. The precipitate was removed by filtration and the filtrate concentrated in vacuo to provide 3-methoxy-2,5,6,7-tetrahydro-1,4-oxazepine (0.94 g, 80%) as a clear oil that was used without further purification.

후처리

  1. customThe reaction was quenched by addition of 1.70 mL saturated aqueous K2CO3
  2. stirringthe mixture was vigorously stirred for 15 minutes
  3. customThe precipitate was removed by filtration
  4. concentrationthe filtrate concentrated in vacuo

출처 및 근거

ORD 기록
ord-a6e58ccf17d14ce0bfebae563c768f00
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835422B2

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