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

HRID 1073002노트

반응식

HRID 1073002 반응식
[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

참가 물질

6

반응물 2

HCID 516951Monobasic potassium phosphateHCID 22047043HCID 22047043, 화합물

생성물 1

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

시약·촉매·용매 3

HCID 962Water용매HCID 6386tert-Butanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-14f67986a2bc47e6805b908003b1d679
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06911543B2

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