Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) → HCID 54228902、化合物

HRID 75120ノート

反応式

HRID 75120 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 54228902HCID 54228902、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a6e58ccf17d14ce0bfebae563c768f00
出典データセット
uspto-grants-2014_09
特許番号
US08835422B2

反応ノート

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