Dimethylformamide → 2-(3-Chlorophenoxymethyl)-alpha-methoxyiminobenzyl chloride

HRID 1387328ノート

反応式

HRID 1387328 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.CN(C)C=O.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:21][C:22]1[CH:32]=[CH:31][CH:30]=[CH:29][C:23]=1[C:24]([Cl:28])=[N:25][O:26][CH3:27]>CCOCC>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:21][C:22]1[CH:32]=[CH:31][CH:30]=[CH:29][C:23]=1[C:24]([Cl:28])=[N:25][O:26][CH3:27]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 79333-ChlorophenolHCID 11430Potassium CarbonateHCID 539269502-Chloromethyl-alpha-methoxyiminobenzyl chloride

生成物 1

HCID 544326462-(3-Chlorophenoxymethyl)-alpha-methoxyiminobenzyl chloride収率 91.2%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

3-Chlorophenol (3.09 g, 0.024 mol), N,N-dimethylforamide (20 ml) and potassium carbonate (4.15 g, 0.03 mol) were added to 2-chloromethyl-α-methoxyiminobenzyl chloride (4.36 g, 0.02 mol), and the mixture was stirred at room temperature for 4 days. After completion of the reaction, ether (250 ml) was added, and the mixture was washed with brine (200 ml) twice. The ether layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to give 2-(3-chlorophenoxymethyl)-α-methoxyiminobenzyl chloride (5.66 g, 91.2%) as a colorless oil.

後処理

  1. additionwas added
  2. washthe mixture was washed with brine (200 ml) twice
  3. dry with materialThe ether layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-045a69055c5c428c914e30c917e3faf9
出典データセット
uspto-grants-2001_07
特許番号
US06268312B1

反応ノート

読み込み中…