Hydrochloric Acid → HCID 11066487、化合物

HRID 1707797ノート

反応式

HRID 1707797 の反応式
[CH3:1][C:2]1[CH:21]=[CH:20][CH:19]=[CH:18][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12](=O)[C:13]([O:15][CH3:16])=[O:14].[Cl-].[OH:23][NH3+:24].Cl>CO>[CH3:1][C:2]1[CH:21]=[CH:20][CH:19]=[CH:18][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1/[C:12](=[N:24]\[OH:23])/[C:13]([O:15][CH3:16])=[O:14]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 21645Hydroxylamine HClHCID 11832950Methyl {2-[(2-methylphenoxy)methyl]phenyl}(oxo)acetate

生成物 1

HCID 11066487HCID 11066487、化合物収率 92.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

56.8 g (0.2 mol) of methyl 2-(2-methylphenoxymethyl)phenylglyoxylate and 15.2 g (0.22 mol) of hydroxylammonium chloride in 67.5 ml of methanol are refluxed for 6.5 hours. The resulting mixture (of E- and Z-oximes) is cooled to 0° C. and 14.2 g (0.39 mol) of hydrogen chloride are passed in, and the mixture is then stirred at 25° C. for 5 hours. The solvent is removed by distillation under reduced pressure, the residue is taken up in diethyl ether, and the solution is washed with water, dried over sodium sulfate and evaporated to dryness. 55.3 g of solid E isomer (melting point 115° C.) are obtained.

後処理

  1. customThe solvent is removed by distillation under reduced pressure
  2. washthe solution is washed with water
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness

出典と根拠

ORDレコード
ord-2e18f7df529347228adf1335ae8cbf11
出典データセット
uspto-grants-1994_10
特許番号
US05354883

反応ノート

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