Dimethyl Sulfate → 5-Methoxy-2,3,6,7-tetrahydro-1,4-oxazepine

HRID 75117ノート

反応式

HRID 75117 の反応式
[O:1]1[CH2:7][CH2:6][C:5](=[O:8])[NH:4][CH2:3][CH2:2]1.S(OC)(O[CH3:13])(=O)=O.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[CH3:13][O:8][C:5]1=[N:4][CH2:3][CH2:2][O:1][CH2:7][CH2:6]1

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 70230201,4-Oxazepan-5-one

生成物 1

HCID 580541675-Methoxy-2,3,6,7-tetrahydro-1,4-oxazepine収率 97.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
150 °C

実験手順

To a solution of 1,4-oxazepan-5-one (0.091 g, 0.793 mmol) in DCM (2 mL) in a screw-cap vial was added dimethyl sulfate (0.1 g, 0.793 mmol) to give a colorless solution. The reaction was heated to 150° C. for 5 minutes. Potassium carbonate (200 mg) was added and the vial was capped and shaken. The reaction was filtered through a glass frit and solvent was removed under reduced pressure to give a clear oil (100 mg) that was used without further purification. LCMS (+ESI) m/z: 130.2 [M+H]+.

後処理

  1. customto give a colorless solution
  2. customthe vial was capped
  3. filtrationThe reaction was filtered through a glass frit and solvent
  4. customwas removed under reduced pressure

出典と根拠

ORDレコード
ord-d76880bf2f724c67a065819467d05dd1
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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