Hydrogen Bromide → Benzo[d]isothiazol-4-ol

HRID 1863212노트

반응식

HRID 1863212 반응식
C[O:2][C:3]1[C:8]2[CH:9]=[N:10][S:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.Br>C(O)(=O)C.[Ta]>[OH:2][C:3]1[C:8]2[CH:9]=[N:10][S:11][C:7]=2[CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 2

HCID 260Hydrogen BromideHCID 193843524-Methoxybenzo[d]isothiazole

생성물 1

HCID 135741992Benzo[d]isothiazol-4-ol수율 69.9%

시약·촉매·용매 2

HCID 23956Tantalum촉매HCID 176Acetic Acid용매

실험 절차

50 g of 4-methoxy-1,2-benzisothiazole are suspended in 700 ml of acetic acid containing 10% by weight of hydrogen bromide and 5 g of red phosphorus, and the suspension is heated for 30 hours at 100° C. in a tantalum autoclave. After cooling, the material discharged from the autoclave is concentrated under reduced pressure and the residue is partitioned between methylene chloride and 2 N sodium hydroxide solution. The water phase is filtered to remove insoluble matter, washed with methylene chloride, acidified with hydrochloric acid and then repeatedly extracted with methylene chloride. The combined extracts are dried over magnesium sulfate and then concentrated under reduced pressure. 32 g (65% of theory) of 4-hydroxy-1,2-benzisothiazole of melting point 133°-134° C. are obtained. C7H5ONS (151)

후처리

  1. temperatureAfter cooling
  2. concentrationis concentrated under reduced pressure
  3. customthe residue is partitioned between methylene chloride and 2 N sodium hydroxide solution
  4. filtrationThe water phase is filtered
  5. customto remove insoluble matter
  6. washwashed with methylene chloride
  7. extractionrepeatedly extracted with methylene chloride
  8. dry with materialThe combined extracts are dried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a77ed7f958354c48a61d3acb6cd3372c
출처 데이터셋
uspto-grants-1979_09
특허 번호
US04168317

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