Methanol → 7-Bromofuro[3,2-c]pyridin-4(5H)-one

HRID 557172

반응식

HRID 557172 반응식
[Br:1]N1C(=O)CCC1=O.[O:9]1[C:17]2[CH:16]=[CH:15][NH:14][C:13](=[O:18])[C:12]=2[CH:11]=[CH:10]1.CO>C(#N)C>[Br:1][C:16]1[C:17]2[O:9][CH:10]=[CH:11][C:12]=2[C:13](=[O:18])[NH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 67184N-bromobutanimideHCID 2887464H,5H-furo(3,2-c)pyridin-4-one

생성물 1

HCID 179855277-Bromofuro[3,2-c]pyridin-4(5H)-one

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

Add N-bromosuccinimide (63.16 g, 354.9 mmol) as a solution in anhydrous acetonitrile (480 mL) to a suspension of 5H-furo[3,2-c]pyridin-4-one (36.9 g, 273 mmol) in anhydrous acetonitrile (740 mL) at 0° C. over 1 hour. Warm to room temperature, add anhydrous methyl alcohol (1.5 L) and stir at room temperature for 18 hours. Quench with water (20 ml) and saturated sodium bicarbonate (20 mL), concentrate to a volume of 1.3 liters, and pour into water (1.3 L). Collection of the precipitate by filtration and drying (vacuum oven 2 days 40-60° C.) gives the title compound as an off-white solid.

후처리

  1. customQuench with water (20 ml) and saturated sodium bicarbonate (20 mL)
  2. concentrationconcentrate to a volume of 1.3 liters
  3. additionpour into water (1.3 L)
  4. customCollection of the precipitate
  5. filtrationby filtration
  6. customdrying (vacuum oven 2 days 40-60° C.)

출처 및 근거

ORD 기록
ord-9bd1f2e713f14c15b1a56ea1de3a101f
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08058425B2

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