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

HRID 325357

反応式

HRID 325357 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 8423(+-)-3,4-Dimethoxyamphetamine収率 96.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-f82ea9512e454fe19c8b6291f86f5b76
出典データセット
uspto-grants-1984_04
特許番号
US04440774

関連ノート

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