Monobasic potassium phosphate → 3-Bromofuro[2,3-c]pyridine-5-carboxylic acid

HRID 1073002ノート

反応式

HRID 1073002 の反応式
[Br:1][C:2]1[C:10]2[C:5](=[CH:6][N:7]=[C:8]([CH:11]=[O:12])[CH:9]=2)[O:4][CH:3]=1.[OH:13]P([O-])(O)=O.[K+]>C1COCC1.CC(O)(C)C.O>[Br:1][C:2]1[C:10]2[C:5](=[CH:6][N:7]=[C:8]([C:11]([OH:13])=[O:12])[CH:9]=2)[O:4][CH:3]=1

参加物

6

反応物 2

HCID 516951Monobasic potassium phosphateHCID 22047043HCID 22047043、化合物

生成物 1

HCID 220476273-Bromofuro[2,3-c]pyridine-5-carboxylic acid収率 100.9%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6386tert-Butanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

3-Bromofuro[2,3-c]pyridine-5-carbaldehyde (3.26 g, 14.42 mmol) is dissolved in THF (100 mL)/t-BuOH (50 mL)/H2O (50 mL), treated with a single portion of NaOCl2 (4.89 g, 43.3 mmol) and KH2PO4 (3.92 g, 28.8 mmol) and stirred at rt for 18 h. The white solid is collected via filtration and the filtrate is concentrated in vacuo to dryness. The residue is suspended in water (25 mL), acidified to pH 2 with concentrated HCl and the resulting solid collected via filtration. The collected solids are dried in a vacuum oven at 50° C. for 18 h and combined to afford 3.52 g (99%) of 3-bromofuro[2,3-c]pyridine-5-carboxylic acid as a white solid. MS (EI) m/z: 241 (M+).

後処理

  1. filtrationThe white solid is collected via filtration
  2. concentrationthe filtrate is concentrated in vacuo to dryness
  3. filtrationthe resulting solid collected via filtration
  4. customThe collected solids are dried in a vacuum oven at 50° C. for 18 h

出典と根拠

ORDレコード
ord-14f67986a2bc47e6805b908003b1d679
出典データセット
uspto-grants-2005_06
特許番号
US06911543B2

反応ノート

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