5-Bromosalicylhydroxamic acid → HCID 178518981、化合物

HRID 1482863ノート

反応式

HRID 1482863 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([OH:12])=[C:6]([CH:11]=1)[C:7]([NH:9]O)=[O:8].C(N1C=CN=C1)(N1C=CN=C1)=O>C1COCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:12][N:9]=[C:7]([OH:8])[C:6]=2[CH:11]=1

参加物

4

反応物 2

HCID 220465-Bromosalicylhydroxamic acidHCID 682631,1'-Carbonyldiimidazole

生成物 1

HCID 178518981HCID 178518981、化合物収率 97.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5-bromo-N,2-dihydroxybenzamide (4.12 g, 17.76 mmol) was suspended in 100 mL THF. Carbonyldiimidazole (5.76 g, 35.5 mmol) was added and the mixture was heated under reflux for three hours. The solvent was evaporated under vacuum, 100 mL water was added and the solution was acidified to pH 1 with 1N HCl under rapid stirring. The formed precipitate was filtered, washed with water and dried, giving 5-bromobenzo[d]isoxazol-3-ol (3.71 g, 17.3 mmol) as off-white solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for three hours
  3. customThe solvent was evaporated under vacuum, 100 mL water
  4. additionwas added
  5. filtrationThe formed precipitate was filtered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-81ebe21a11a443078bdedfaad161087c
出典データセット
uspto-grants-2016_08
特許番号
US09416115B2

反応ノート

読み込み中…