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

HRID 1074426노트

반응식

HRID 1074426 반응식
[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

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 21618620HCID 21618620, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b74ceb59b9fe481c820a56cb79eeaeff
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04391805

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