Phenazopyridine hydrochloride → Phenazopyridine

HRID 2063231노트

반응식

HRID 2063231 반응식
C(=O)([O-])[O-].[K+].[K+].[CH:7]1[CH:8]=[CH:9][C:10]([N:13]=[N:14][C:15]2[CH:16]=[CH:17][C:18]([NH2:22])=[N:19][C:20]=2[NH2:21])=[CH:11][CH:12]=1.Cl.C(OCC)(=O)C>O>[CH:7]1[CH:12]=[CH:11][C:10]([N:13]=[N:14][C:15]2[CH:16]=[CH:17][C:18]([NH2:22])=[N:19][C:20]=2[NH2:21])=[CH:9][CH:8]=1

참가 물질

5

반응물 3

HCID 8691Phenazopyridine hydrochlorideHCID 8857Ethyl AcetateHCID 11430Potassium Carbonate

생성물 1

HCID 4756Phenazopyridine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 27.6 grams (200 mmol) of potassium carbonate in 200 mL of water was added 20.0 grams (80 mmol) of phenazopyridine hydrochloride followed by 200 mL of ethyl acetate. The mixture was stirred at room temperature for 30 minutes. The layers were separated and the aqueous layer was extracted one time with 100 mL of ethyl acetate. The ethyl acetate layer was dried over sodium sulfate, and filtered. The filtrate was concentrated under diminished pressure and the product was dried under vacuum at room temperature to give an orange solid: yield 15.1 grams (92%). 1H NMR (300 MHz, CDCl3) δ 4.80 (br s, 4H), 6.06 (d, 1H), 7.34 (m, 1H), 7.48 (m, 2H), 7.76 (m, 2H), and 7.93 (d, 1H).

후처리

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted one time with 100 mL of ethyl acetate
  3. dry with materialThe ethyl acetate layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under diminished pressure
  6. customthe product was dried under vacuum at room temperature
  7. customto give an orange solid

출처 및 근거

ORD 기록
ord-0c5079e1206b451c8de60eb45ad9c3dc
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288365B2

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