Hydrochloric Acid → Hydroxyamfetamine

HRID 6729

反応式

HRID 6729 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=O)[CH3:10])=[CH:4][CH:3]=1.C([O-])(=O)C.[NH4+].C([BH3-])#[N:18].[Na+].Cl>CO>[NH2:18][CH:9]([CH3:10])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([OH:1])=[CH:3][CH:4]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 70192744-Hydroxyphenylacetone

生成物 1

HCID 3651Hydroxyamfetamine収率 56.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 4-hydroxyphenylacetone (0.5 g, Avocado, U.K.) and ammonium acetate (2.54 g, Aldrich, U.S.A.) in 10 mL methanol was added 0.17 g of sodium cyanoborohydride (Aldrich, U.S.A.). After stirring for 72 h at rt, concentrated hydrochloric acid was added dropwise until the solution reached pH 2. The solvent was evaporated and the resulting residue was dissolved in water, then extracted 3 times with diethyl ether. The aqueous layer was neutralized to pH 8 by the addition of potassium hydroxide and extracted with diethyl ether. The basic ether layer was dried over sodium sulfate and the solvent was removed in vacuo to give 0.23 g of 4-(2-amino-propyl)-phenol.

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe resulting residue was dissolved in water
  3. extractionextracted 3 times with diethyl ether
  4. additionThe aqueous layer was neutralized to pH 8 by the addition of potassium hydroxide
  5. extractionextracted with diethyl ether
  6. dry with materialThe basic ether layer was dried over sodium sulfate
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-66b12eb350804cde8d3d3a98c42becda
出典データセット
uspto-grants-2006_08
特許番号
US07084154B2

関連ノート

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