5-Bromosalicylhydroxamic acid → HCID 178518981, 화합물

HRID 1482863노트

반응식

HRID 1482863 반응식
[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

참가 물질

4

반응물 2

HCID 220465-Bromosalicylhydroxamic acidHCID 682631,1'-Carbonyldiimidazole

생성물 1

HCID 178518981HCID 178518981, 화합물수율 97.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-81ebe21a11a443078bdedfaad161087c
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09416115B2

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