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

HRID 358720
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인쇄 미리보기

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HRID 358720 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-533814242a3344c1aa2444826b05225a
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04997840

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