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Methane → 1-(2H-1,3-Benzodioxol-5-yl)-2-methylpropan-2-amine

HRID 616258
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HRID 616258 반응식
[CH3:1][C:2]([N+:15]([O-])=O)([CH3:14])[CH:3](Cl)[C:4]1[CH:9]=[CH:8][C:7]2[O:10][CH2:11][O:12][C:6]=2[CH:5]=1.C([O-])(=O)C.[Na+].C.[H][H]>C(O)(=O)C.[Pt]=O>[CH3:14][C:2]([NH2:15])([CH3:1])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]2[O:10][CH2:11][O:12][C:6]=2[CH:5]=1
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참가 물질

7

반응물 4

HCID 297MethaneHCID 517045Sodium AcetateHCID 234548395-(1-Chloro-2-methyl-2-nitropropyl)-2H-1,3-benzodioxoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 130205981-(2H-1,3-Benzodioxol-5-yl)-2-methylpropan-2-amine

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)
촉매
HCID 176Acetic Acid용매

실험 절차

A mixture of 51.52 g (0.2 mole) of 1,1-dimethyl-2-chloro-2-(3,4-methylenedioxyphenyl)nitroethane, 2.0 g of 83.8 weight % purity platinum oxide, 18.0 g (0.22 mole) of sodium acetate and 4.0 g of "Darco" in 96 ml of acetic acid and 500 ml of SDA-30 was stirred under a hydrogen atmosphere at 1000 p.s.i. and 100° C for a period of 5 hours, after which uptake of hydrogen ceased. The solution was cooled and filtered, and the filtrate was concentrated to an oil which was treated with 400 ml of water. The mixture was extracted twice with ether, after which the aqueous layer was made alkaline by addition of 20% aqueous sodium hydroxide and extracted four times with chloroform. The combined extracts were filtered through "Dicalite" (Trade Mark), washed with water, dried and concentrated to a light yellow oil which was distilled using a 2" 19.38 distillation column to give 1,1-dimethyl-2-(3,4-methylenedioxyphenyl)ethylamine as a clear colourless oil, b.p. 68°-85° C, 0.06-0.04 mm Hg (Yield 24.4 g, 63.2%)

후처리

  1. temperatureThe solution was cooled
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated to an oil which
  4. additionwas treated with 400 ml of water
  5. extractionThe mixture was extracted twice with ether
  6. additionby addition of 20% aqueous sodium hydroxide
  7. extractionextracted four times with chloroform
  8. filtrationThe combined extracts were filtered through "Dicalite" (Trade Mark)
  9. washwashed with water
  10. customdried
  11. concentrationconcentrated to a light yellow oil which
  12. distillationwas distilled
  13. distillationa 2" 19.38 distillation column

출처 및 근거

ORD 기록
ord-58e9a8a5dff44a33b9c551c0dddb7695
출처 데이터셋
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04073798

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