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

HRID 225503

반응식

HRID 225503 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d2829c2fd933447e93829e3a197b0e72
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557105B2

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