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Dimethyl Sulfate → HCID 86647569, 화합물

HRID 1664079
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HRID 1664079 반응식
[CH3:1][N:2]([CH3:16])[CH2:3][CH2:4][CH2:5][N:6]([C:8]1[CH:15]=[CH:14]C=[CH:12][C:9]=1C=O)[CH3:7].[S:17]([O:22]C)(O[CH3:21])(=[O:19])=[O:18].[C:24]([O:27][CH2:28][CH3:29])(=O)C>ClCCl>[CH3:24][S:17]([O-:22])(=[O:19])=[O:18].[CH:28]([C:29]1[CH:12]=[CH:9][C:8]([N:6]([CH3:7])[CH2:5][CH2:4][CH2:3][N+:2]([CH3:1])([CH3:16])[CH3:21])=[CH:15][CH:14]=1)=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 8857Ethyl AcetateHCID 63695083HCID 63695083, 화합물

생성물 1

HCID 86647569HCID 86647569, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

5 g of [[3-(dimethylamino)propyl](methyl)amino]benzaldehyde are diluted in 15 ml of dichloromethane. 2.36 ml of dimethyl sulphate diluted in 10 ml of dichloromethane are gradually added. The mixture is refluxed for 4 h and then cooled to ambient temperature and poured into 100 ml of ethyl acetate. The brown oil formed is separated by settling out, washed with 100 ml of EtOAc, taken up in 200 ml of methanol and concentrated under vacuum. It is subsequently dissolved in a saturated solution of sodium bicarbonate and of sodium chloride and extracted with butanol. The butanol phase is concentrated under vacuum and dried under vacuum in the presence of P2O5, and the product is then used for the subsequent step.

후처리

  1. additionare gradually added
  2. temperatureThe mixture is refluxed for 4 h
  3. customThe brown oil formed
  4. customis separated
  5. washwashed with 100 ml of EtOAc
  6. concentrationconcentrated under vacuum
  7. dissolutionIt is subsequently dissolved in a saturated solution of sodium bicarbonate and of sodium chloride
  8. extractionextracted with butanol
  9. concentrationThe butanol phase is concentrated under vacuum
  10. dry with materialdried under vacuum in the presence of P2O5

출처 및 근거

ORD 기록
ord-08d558de09714ef4b8b2e4fa0121159f
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08038732B2

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