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Methyl chloroformate → HCID 20477998, 화합물

HRID 904893
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HRID 904893 반응식
[CH3:1][N:2]([CH3:16])[CH2:3][CH2:4][NH:5][C:6]1[C:11]([C:12]#[N:13])=[C:10]([CH3:14])[CH:9]=[C:8]([CH3:15])[N:7]=1.Cl[C:18]([O:20][CH3:21])=[O:19]>C1C=CC=CC=1>[C:12]([C:11]1[C:6]([N:5]([CH2:4][CH2:3][N:2]([CH3:16])[CH3:1])[C:18](=[O:19])[O:20][CH3:21])=[N:7][C:8]([CH3:15])=[CH:9][C:10]=1[CH3:14])#[N:13]
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참가 물질

4

반응물 2

HCID 6586Methyl chloroformateHCID 34118773-Pyridinecarbonitrile, 2-[[2-(dimethylamino)ethyl]amino]-4,6-dimethyl-

생성물 1

HCID 20477998HCID 20477998, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution of N,N-dimethyl-N'-(3-cyano-4,6-dimethyl-2-pyridyl)-1,2-diaminoethane (13.5 g, 62 mmol) in dry benzene (150 ml) is added methyl chloroformate (7.1 ml, 92 mmol) and then the resulting mixture is refluxed for 11/2 hours. This mixture is evaporated to dryness and the residue dissolved in water, washed with methylene chloride, made basic with sodium carbonate and the product extracted into methylene chloride. Upon evaporation of the solvent there is obtained 16.6 g of oily title B product.

후처리

  1. temperaturethe resulting mixture is refluxed for 11/2 hours
  2. customThis mixture is evaporated to dryness
  3. dissolutionthe residue dissolved in water
  4. washwashed with methylene chloride
  5. extractionthe product extracted into methylene chloride
  6. customUpon evaporation of the solvent there
  7. customis obtained 16.6 g of oily title B product

출처 및 근거

ORD 기록
ord-b96706175e974d22832a3403f14119e4
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04420615

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