Hydrochloric Acid → 4-((3-Oxopiperazin-1-yl)methyl)benzoic acid

HRID 225503

反応式

HRID 225503 の反応式
BrC[C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][C:13]1=[O:18].[C:19](=O)([O-])[O-].[K+].[K+].Cl>CO>[O:18]=[C:13]1[NH:12][CH2:17][CH2:16][N:15]([CH2:19][C:11]2[CH:3]=[CH:4][C:5]([C:6]([OH:8])=[O:7])=[CH:9][CH:10]=2)[CH2:14]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 231360Piperazin-2-oneHCID 2456503-(Bromomethyl)benzoic acid

生成物 1

HCID 167770994-((3-Oxopiperazin-1-yl)methyl)benzoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 3-bromomethylbenzoic acid (4.30 g, 20 mmol), piperazin-2-one (2.0 g, 20 mmol) and powdered potassium carbonate (2.76 g, 20 mmol) in methanol (50 mL) is stirred for 17 hours at room temperature. The resulting mixture is filtered and the solvent is evaporated off under reduced pressure to give a residue which is treated with hydrochloric acid (80 mL of 0.25 M) and stirred for 5 min. The precipitated product is filtered, washed with water, dried and recrystallised from methanol to give the title compound as a cream crystalline solid.

後処理

  1. filtrationThe resulting mixture is filtered
  2. customthe solvent is evaporated off under reduced pressure
  3. customto give a residue which
  4. stirringstirred for 5 min
  5. filtrationThe precipitated product is filtered
  6. washwashed with water
  7. customdried
  8. customrecrystallised from methanol

出典と根拠

ORDレコード
ord-d2829c2fd933447e93829e3a197b0e72
出典データセット
uspto-grants-2009_07
特許番号
US07557105B2

関連ノート

読み込み中…