Phenazopyridine hydrochloride → Phenazopyridine

HRID 2063231ノート

反応式

HRID 2063231 の反応式
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

参加物

5

反応物 3

HCID 8691Phenazopyridine hydrochlorideHCID 8857Ethyl AcetateHCID 11430Potassium Carbonate

生成物 1

HCID 4756Phenazopyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0c5079e1206b451c8de60eb45ad9c3dc
出典データセット
uspto-grants-2012_10
特許番号
US08288365B2

反応ノート

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