Formaldehyde → ethyl 2-[4-{N-(4-chlorophenyl)-N-methylaminomethyl}phenoxy]-2-methylpropionate

HRID 2058095ノート

反応式

HRID 2058095 の反応式
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([NH:6][CH2:7][C:8]2[CH:22]=[CH:21][C:11]([O:12][C:13]([CH3:20])([CH3:19])[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[CH2:25]=O>C(O)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:6]([CH2:7][C:8]2[CH:9]=[CH:10][C:11]([O:12][C:13]([CH3:19])([CH3:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:21][CH:22]=2)[CH3:25])=[CH:23][CH:24]=1

参加物

4

反応物 2

HCID 712FormaldehydeHCID 20329838Ethyl 2-[4-(4-chloroanilinomethyl)phenoxy]-2-methylpropionate

生成物 1

HCID 20329844ethyl 2-[4-{N-(4-chlorophenyl)-N-methylaminomethyl}phenoxy]-2-methylpropionate

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

To 2.9 g of ethyl 2-[4-(4-chloroanilinomethyl)phenoxy]-2-methylpropionate are added 10 ml of formaldehyde and 20 ml of formic acid to prepare a solution, which is stirred at room temperature for 30 minutes and then at 50° C. for 1 hour. The formaldehyde and formic acid are distilled off from the reaction mixture under reduced pressure, and ethanol is added to the residue. After filtering off the insolubles from the resulting solution, the ethanol is distilled off from the filtrate. The resulting oily residue is dissolved in ether, washed with water and dried. The ether is distilled off from the dried solution to given an oily residue (2.8 g), which is purified by silica gel column chromatography, using chloroform as an eluent to give 2.3 g of ethyl 2-[4-{N-(4-chlorophenyl)-N-methylaminomethyl}phenoxy]-2-methylpropionate, an oily product.

後処理

  1. customto prepare a solution, which
  2. waitat 50° C. for 1 hour
  3. distillationThe formaldehyde and formic acid are distilled off from the reaction mixture under reduced pressure, and ethanol
  4. additionis added to the residue
  5. filtrationAfter filtering off the insolubles from the resulting solution
  6. distillationthe ethanol is distilled off from the filtrate
  7. dissolutionThe resulting oily residue is dissolved in ether
  8. washwashed with water
  9. customdried
  10. distillationThe ether is distilled off from the dried solution
  11. customis purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-59a00eee5db9437196406c66ff4e376b
出典データセット
uspto-grants-1980_07
特許番号
US04214094

反応ノート

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