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Formic Acid → N-[2-(Chloroacetyl)phenyl]-N-methylformamide

HRID 358720
ノート
印刷プレビュー

反応式

HRID 358720 の反応式
[CH:1]([OH:3])=O.C(OC(=O)C)(=O)C.[Cl:11][CH2:12][C:13]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[NH:21][CH3:22])=[O:14].C(=O)(O)[O-].[Na+]>ClCCl.O>[Cl:11][CH2:12][C:13]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:21]([CH3:22])[CH:1]=[O:3])=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 198249382-Chloro-1-[2-(methylamino)phenyl]ethanone

生成物 1

HCID 23128087N-[2-(Chloroacetyl)phenyl]-N-methylformamide

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

A mixture of formic acid (2.3 ml) and acetic anhydride (3.6 ml) was heated at 50 to 60° for 2 hours, cooled to 0 to 5° and dichloromethane (10 ml) added. A solution of 2-chloro-2'-(methylamino)acetophenone (1.6 g) in dichloromethane (25 ml) was added and the solution then stirred at 10°-20° for 3 hours. The solution was cooled to 0 to 5° and water (50 ml) followed by aqueous sodium bicarbonate (1M, 50 ml) was added. The layers were separated and the aqueous layer was extracted with dichloromethane (50 ml). The combined dichloromethane layer and extract were dried over magnesium sulphate and the solvent was removed by distillation to give the novel compound 2'-(2-chloro-acetyl)-N-methylformanilide in the form of an oil.

後処理

  1. temperaturewas heated at 50 to 60° for 2 hours
  2. temperaturecooled to 0 to 5°
  3. temperatureThe solution was cooled to 0 to 5°
  4. additionwas added
  5. customThe layers were separated
  6. extractionthe aqueous layer was extracted with dichloromethane (50 ml)
  7. extractionThe combined dichloromethane layer and extract
  8. dry with materialwere dried over magnesium sulphate
  9. customthe solvent was removed by distillation

出典と根拠

ORDレコード
ord-533814242a3344c1aa2444826b05225a
出典データセット
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04997840

反応ノート

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