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

HRID 368828

反応式

HRID 368828 の反応式
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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9e48444c65764aceb8285e138d0b3932
出典データセット
uspto-grants-2000_10
特許番号
US06133446

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