Hydrochloric Acid → (+-)-3,4-Dimethoxyamphetamine

HRID 325357

반응식

HRID 325357 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][C:12](=O)[CH3:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C([BH3-])#[N:16].[Na+].Cl>CO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([NH2:16])[CH3:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 698962-Propanone, 1-(3,4-dimethoxyphenyl)-HCID 5003444Sodium cyanoborohydride

생성물 1

HCID 8423(+-)-3,4-Dimethoxyamphetamine수율 96.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 3,4-dimethoxyphenylacetone (51.1 g., 0.26 m.) is dissolved in methanol (780 ml.), sodium cyanoborohydride (11.3 g., 0.18 m) is added and the mixture is stirred at room temperature for 67 hours. The reaction mixture is adjusted to pH 2 with concentrated HCl and the solvent is evaporated under reduced pressure. The residue is dissolved in H2O (250 ml.), the aqueous layer is extracted with ether (3×) and then rendered alkaline with KOH and extracted with CH2Cl2 (3×). After drying, the solvent is evaporated under reduced pressure and the product is distilled at 112°-5°/0.5 mm. to yield (VIII) (33.88 g., 67%).

후처리

  1. customthe solvent is evaporated under reduced pressure
  2. dissolutionThe residue is dissolved in H2O (250 ml.)
  3. extractionthe aqueous layer is extracted with ether (3×)
  4. extractionextracted with CH2Cl2 (3×)
  5. customAfter drying
  6. customthe solvent is evaporated under reduced pressure
  7. distillationthe product is distilled at 112°-5°/0.5 mm

출처 및 근거

ORD 기록
ord-f82ea9512e454fe19c8b6291f86f5b76
출처 데이터셋
uspto-grants-1984_04
특허 번호
US04440774

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