Acetic Acid → 7-Chloro-2,3-dihydrobenzo[d]isothiazole 1,1-Dioxide

HRID 1251945노트

반응식

HRID 1251945 반응식
[Cl:1][C:2]1[C:10]2[S:9](=[O:12])(=[O:11])[N:8]=[CH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+].C(O)(=O)C>C(O)C>[Cl:1][C:2]1[C:10]2[S:9](=[O:12])(=[O:11])[NH:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 4311764Sodium borohydrideHCID 136863097-Chloro-1,2-benzisothiazole-1,1-dioxide

생성물 1

HCID 136863107-Chloro-2,3-dihydrobenzo[d]isothiazole 1,1-Dioxide수율 97.4%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
0 °C

실험 절차

A suspension of 17.9 g of 7-chloro-1,2-benzisothiazole-1,1-dioxide in 180 ml of absolute ethanol was cooled to 0° C. and treated with 3.33 g of sodium borohydride at such a rate that the temperature remained below 5° C. The mixture was warmed to room temperature for 30 minutes, recooled to 0° C. and treated with glacial acetic acid to destroy excess hydride. The mixture was concentrated to dryness, the resulting solid suspended in water, filtered, washed with water and dried in vacuo at 50° C. for 16 hours to give 17.6 g of the title compound as a white powder, m.p. 159°-161° C.

후처리

  1. customremained below 5° C
  2. temperatureThe mixture was warmed to room temperature for 30 minutes
  3. customrecooled to 0° C.
  4. customto destroy excess hydride
  5. concentrationThe mixture was concentrated to dryness
  6. filtrationfiltered
  7. washwashed with water
  8. customdried in vacuo at 50° C. for 16 hours

출처 및 근거

ORD 기록
ord-e82f3094ccf743c68a767d17824a216c
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04741761

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