Water → 3-(4-methylbenzyloxyimino)-2-methoxyimino-N,N-dimethylbutyramide

HRID 1069195

反応式

HRID 1069195 の反応式
[OH:1][N:2]=[C:3]([CH3:13])[C:4](=[N:10][O:11][CH3:12])[C:5]([N:7]([CH3:9])[CH3:8])=[O:6].[CH3:14][C:15]1[CH:22]=[CH:21][C:18]([CH2:19]Cl)=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].O>CC(C)=O>[CH3:14][C:15]1[CH:22]=[CH:21][C:18]([CH2:19][O:1][N:2]=[C:3]([CH3:13])[C:4](=[N:10][O:11][CH3:12])[C:5]([N:7]([CH3:8])[CH3:9])=[O:6])=[CH:17][CH:16]=1

参加物

6

反応物 4

HCID 962WaterHCID 77224-Methylbenzyl chlorideHCID 11430Potassium CarbonateHCID 1361176603-hydroxyimino-2-methoxyimino-N,N-dimethylbutyramide

生成物 1

HCID 536799603-(4-methylbenzyloxyimino)-2-methoxyimino-N,N-dimethylbutyramide収率 96.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 600 mg (3.2 mmol) of 3-hydroxyimino-2-methoxyimino-N,N-dimethylbutyramide in 20 ml of acetone, 500 mg (3.5 mmol) of 4-methylbenzylchloride and 660 mg (4.8 mmol) of potassium carbonate were added and the mixture was heated under reflux for 16 hours. The reaction mixture was combined with 30 ml of water and extracted three times with 30 ml of diethylether. After washing with water and a saturated aqueous sodium chloride, the mixture was dried over with anhydrous magnesium sulfate and then the solvent was distilled off. The residue thus obtained was purified by a column chromatography on a silica gel (n-hexane/ethyl acetate) to obtain 900 mg (yield: 96%) of 3-(4-methylbenzyloxyimino)-2-methoxyimino-N,N-dimethylbutyramide as a colorless crystal.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 16 hours
  3. extractionextracted three times with 30 ml of diethylether
  4. washAfter washing with water
  5. dry with materiala saturated aqueous sodium chloride, the mixture was dried over with anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off
  7. customThe residue thus obtained
  8. customwas purified by a column chromatography on a silica gel (n-hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-4439910297a7458ab185eeef33af6f63
出典データセット
uspto-grants-2001_06
特許番号
US06251949B1

関連ノート

読み込み中…