Potassium Cyanide → 2-Amino-2-cyano-5-methoxy-1,2,3,4-tetrahydronaphthalene

HRID 128713

反応式

HRID 128713 の反応式
[C-:1]#[N:2].[K+].[Cl-].[NH4+:5].[CH3:6][O:7][C:8]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:9]=1[CH2:10][CH2:11][C:12](=O)[CH2:13]2>C(O)C.O>[NH2:5][C:12]1([C:1]#[N:2])[CH2:11][CH2:10][C:9]2[C:14](=[CH:15][CH:16]=[CH:17][C:8]=2[O:7][CH3:6])[CH2:13]1

参加物

6

反応物 3

HCID 9032Potassium CyanideHCID 25517Ammonium ChlorideHCID 2591945-Methoxy-2-tetralone

生成物 1

HCID 99904312-Amino-2-cyano-5-methoxy-1,2,3,4-tetrahydronaphthalene

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

112 mmol of potassium cyanide and 116 mmol of ammonium chloride ate added successively to a solution, maintained under nitrogen and with stirring, containing 110 mmol of 5-methoxy-3,4-dihydronaphthalen-2(1H)-one in 90 ml of ethanol and 50 ml of water. The whole mixture is stirred for 20 hours at 20° C. and then concentrated under vacuum. The residue is taken up in 200 ml of ethyl acetate. This phase is then washed with water and extracted with 1N hydrochloric acid. The acid phase is basified with 35% sodium hydroxide solution and extracted with methyl acetate. The combined organic phases are dried and evaporated under vacuum and lead to the expected product in the solid form.

後処理

  1. temperaturemaintained under nitrogen
  2. stirringThe whole mixture is stirred for 20 hours at 20° C.
  3. concentrationconcentrated under vacuum
  4. washThis phase is then washed with water
  5. extractionextracted with 1N hydrochloric acid
  6. extractionextracted with methyl acetate
  7. customThe combined organic phases are dried
  8. customevaporated under vacuum and lead to the expected product in the solid form

出典と根拠

ORDレコード
ord-ba8afc10f72a433885205de1993275b0
出典データセット
uspto-grants-1995_11
特許番号
US05464859

関連ノート

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