Diethyl Ether → N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-alpha-chloroacetanilide

HRID 28040ノート

反応式

HRID 28040 の反応式
[CH2:1]([CH:4]1[CH2:8][O:7][CH:6]([CH2:9][NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2OC)[O:5]1)[CH2:2][CH3:3].[CH2:19]([O:21][CH2:22]C)C.[C:24](=[O:27])([O-])[O-].[Na+].[Na+].[Cl:30]CC(Cl)=O>O>[CH2:1]([CH:4]1[CH2:8][O:7][CH:6]([CH2:9][N:10]([C:24](=[O:27])[CH:19]([O:21][CH3:22])[Cl:30])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[O:5]1)[CH2:2][CH3:3]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 6577Chloroacetyl chlorideHCID 10340Sodium CarbonateHCID 23338370HCID 23338370、化合物

生成物 1

HCID 23338389N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-alpha-chloroacetanilide

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

N-(4-Propyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline (0.25 mole), diethyl ether (30 ml), sodium carbonate (35.5 grams) and water (50 ml) are charged into a glass reaction vessel equipped with stirrer, thermometer and cooling means. The mixture is cooled to about 5° C. and chloroacetyl chloride (0.28 mole) is added dropwise with stirring. After the addition is completed, stirring is continued for 1 hour. After this time the organic phase is separated from the aqueous phase and is filtered. The filtrate is then washed with aqueous sodium carbonate, dried over anhydrous magnesium sulfate and filtered. The filtrate is then stripped of solvent under reduced pressure to yield the desired product N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-α-chloroacetanilide as the residue.

後処理

  1. customequipped with stirrer
  2. temperaturethermometer and cooling means
  3. additionAfter the addition
  4. stirringstirring
  5. customAfter this time the organic phase is separated from the aqueous phase
  6. filtrationis filtered
  7. washThe filtrate is then washed with aqueous sodium carbonate
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-014ae2fa5ffd4701817a05d6204d0400
出典データセット
uspto-grants-1980_09
特許番号
US04225335

反応ノート

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