1-Formyl-4-(2-bromo-4-methoxyphenyl)piperazine → 1-(2-Bromo-4-methoxyphenyl)piperazine

HRID 1417809

반응식

HRID 1417809 반응식
C([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][C:10]=2[Br:17])[CH2:5][CH2:4]1)=O>Cl>[Br:17][C:10]1[CH:11]=[C:12]([O:15][CH3:16])[CH:13]=[CH:14][C:9]=1[N:6]1[CH2:7][CH2:8][NH:3][CH2:4][CH2:5]1

참가 물질

3

반응물 1

HCID 232888181-Formyl-4-(2-bromo-4-methoxyphenyl)piperazine

생성물 1

HCID 232889281-(2-Bromo-4-methoxyphenyl)piperazine

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A mixture of 1-formyl-4-(2-bromo-4-methoxyphenyl)piperazine (VII, 3.92 g, 3.1 mmol) and hydrochloric acid (4N, 70 ml) is heated at 100° for 50 min. The mixture is then concentrated under reduced pressure to remove most of the aqueous hydrochloric acid. Saturated sodium bicarbonate is then cautiously added and the aqueous phase is extracted with dichloromethane. The combined organic phase is backwashed with saline, dried over magnesium sulfate, and concentrated to give 1-(2-bromo-4-methoxyphenyl)piperazine (VIII), NMR (CDCl3) 2.55, 2.95, 3.08, 3.77, 6.83, 7.01, 7.14 δ.

후처리

  1. temperatureis heated at 100° for 50 min
  2. concentrationThe mixture is then concentrated under reduced pressure
  3. customto remove most of the aqueous hydrochloric acid
  4. additionSaturated sodium bicarbonate is then cautiously added
  5. extractionthe aqueous phase is extracted with dichloromethane
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-adba3b0f6a4f4aa382e2cf38ed387201
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05877317

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