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1,2-Dichloroethane → 77640-10-9

HRID 127599
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HRID 127599 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[CH:3]1.[Cl-].[Al+3].[Cl-].[Cl-].C([CH:13]([C:17](Cl)=[O:18])[C:14](Cl)=[O:15])C.[OH2:20].Cl[CH2:22][CH2:23]Cl>ClC(Cl)C>[CH2:22]([O:20][C:17](=[O:18])[CH2:13][C:14](=[O:15])[C:3]1[N:2]([CH3:1])[CH:6]=[CH:5][CH:4]=1)[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 962WaterHCID 73041-MethylpyrroleHCID 6451240Aluminum(III) ChlorideHCID 109209242-Ethylpropanedioyl dichloride

생성물 1

HCID 1035262977640-10-9

시약·촉매·용매 1

HCID 6365
1,1-Dichloroethane
용매

실험 절차

The starting material is prepared as follows: To the solution of 17 g of 1-methylpyrrole in 400 ml of 1,2-dichloroethane is added 28 g of anhydrous aluminum chloride in portions, while stirring and cooling to 10°-15°, followed by 27 g of ethyl malonyl chloride in 50 ml of dichloroethane at such a rate to keep the temperature between 10° and 15°. After stirring for 3.5 hours the temperature is allowed to rise slowly to 32° and the mixture is allowed to stand overnight at room temperature. It is treated with water, shaken, the organic layer separated, washed twice with water, dried and evaporated. The residual dark brown oil is distilled and the fraction boiling at 105-112/0.25 mm Hg collected, to yield the 1-methyl-β-oxo-2-pyrrolpropionic acid ethyl ester.

후처리

  1. customThe starting material is prepared
  2. temperaturecooling to 10°-15°
  3. customthe temperature between 10° and 15°
  4. stirringAfter stirring for 3.5 hours the temperature
  5. customto rise slowly to 32°
  6. stirringshaken
  7. customthe organic layer separated
  8. washwashed twice with water
  9. customdried
  10. customevaporated
  11. distillationThe residual dark brown oil is distilled
  12. customcollected

출처 및 근거

ORD 기록
ord-626e48f60a28482aa9b84ffb09a64300
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04256759

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