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

HRID 557172

反応式

HRID 557172 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

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.

後処理

  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.)

出典と根拠

ORDレコード
ord-9bd1f2e713f14c15b1a56ea1de3a101f
出典データセット
uspto-grants-2011_11
特許番号
US08058425B2

関連ノート

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