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1-Methoxy-2-propanol → 2',6'-Dimethyl-N-(2-Methoxy-1-Methylethoxymethyl) 2-Chloroacetanilide

HRID 466343
ノート
印刷プレビュー

反応式

HRID 466343 の反応式
[CH3:1][C:2]1[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[C:3]=1[N:4]([CH2:9]Cl)[C:5](=[O:8])[CH2:6][Cl:7].[CH3:16][O:17][CH2:18][CH:19]([CH3:21])[OH:20]>C(Cl)CCl>[CH3:1][C:2]1[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[C:3]=1[N:4]([CH2:9][O:20][CH:19]([CH3:21])[CH2:18][O:17][CH3:16])[C:5](=[O:8])[CH2:6][Cl:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 79001-Methoxy-2-propanolHCID 130698822-Chloro-N-(chloromethyl)-N-(2,6-dimethylphenyl)acetamide

生成物 1

HCID 538049682',6'-Dimethyl-N-(2-Methoxy-1-Methylethoxymethyl) 2-Chloroacetanilide収率 99.1%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

About 12.3 g (0.050 mole) of 2',6'-dimethyl-N-(chloromethyl) 2-chloroacetanilide dissolved in twenty (20) ml of ethylene dichloride was added to 22.5 g (0.25 mole) of 2-methoxy-1-methyl ethanol. The solution was allowed to stand one hour at room temperature. Excess alcohol and HCl was removed under vacuum on a rotary evaporator. The residual oil was treated with an additional 22.5 g fresh alcohol for 30 minutes at 60° C. Excess alcohol and HCl was removed as before at 65° C./1 mm Hg. The light yellow oily residue weighed 14.86 g (99.1% yield). Refractive index of the oil, n26D 1.5263. Proton NMR was consistent with structure.

後処理

  1. customExcess alcohol and HCl was removed under vacuum on a rotary evaporator
  2. additionThe residual oil was treated with an additional 22.5 g fresh alcohol for 30 minutes at 60° C
  3. customExcess alcohol and HCl was removed as before at 65° C./1 mm Hg

出典と根拠

ORDレコード
ord-0eb9537c996a4f38abfb6431391683cf
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05155272

反応ノート

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