Hydrogen Bromide → 4-[2-(piperidin-1-yl)ethyl]phenol

HRID 1074426ノート

反応式

HRID 1074426 の反応式
[N:1]1([CH2:7][CH2:8][C:9]2[CH:14]=[CH:13][C:12]([O:15]C)=[CH:11][CH:10]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Br>C(O)(=O)C>[N:1]1([CH2:7][CH2:8][C:9]2[CH:10]=[CH:11][C:12]([OH:15])=[CH:13][CH:14]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 21618620HCID 21618620、化合物

生成物 1

HCID 2611294-[2-(piperidin-1-yl)ethyl]phenol

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 11 g=50 mmoles of 4-(piperidin-1-ylethyl)-anisole in a mixture of 50 ml of glacial acetic acid and 50 ml of 48% strength hydrobromic acid is boiled under reflux for 4 hours, the solution is evaporated in vacuo and the residue is recrystallized from ethanol. This gives 9 g of the hydrobromide, melting point: 265° C. The salt is dissolved in 30 ml of water and the free base is precipitated with concentrated aqueous ammonia solution and is filtered off. This gives 5.5 g (54% of theory), melting point: 168°-169° C.

後処理

  1. temperatureunder reflux for 4 hours
  2. customthe solution is evaporated in vacuo
  3. customthe residue is recrystallized from ethanol
  4. dissolutionThe salt is dissolved in 30 ml of water
  5. customthe free base is precipitated with concentrated aqueous ammonia solution
  6. filtrationis filtered off

出典と根拠

ORDレコード
ord-b74ceb59b9fe481c820a56cb79eeaeff
出典データセット
uspto-grants-1983_07
特許番号
US04391805

反応ノート

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