1,2,3-Benzothiadiazol-7-ylmethanol → Benzo[d][1,2,3]thiadiazole-7-carbaldehyde

HRID 257132

반응식

HRID 257132 반응식
[OH:1][CH2:2][C:3]1[C:11]2[S:10][N:9]=[N:8][C:7]=2[CH:6]=[CH:5][CH:4]=1>C(Cl)(Cl)Cl.[O-2].[O-2].[Mn+4]>[S:10]1[C:11]2[C:3]([CH:2]=[O:1])=[CH:4][CH:5]=[CH:6][C:7]=2[N:8]=[N:9]1

참가 물질

4

반응물 1

HCID 200964331,2,3-Benzothiadiazol-7-ylmethanol

생성물 1

HCID 14835681Benzo[d][1,2,3]thiadiazole-7-carbaldehyde수율 91.5%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매2회HCID 6212Chloroform용매

실험 절차

To a solution of 16.6 g of 7-hydroxymethylbenzo-1,2,3-thiadiazole in 100 ml of chloroform there are introduced with stirring at room temperature 35 g of manganese dioxide, during which process the internal temperature rises briefly to 31° C. When the temperature has dropped again to 25° C., the mixture is heated and refluxed overnight. Another 5 g of manganese dioxide are subsequently added, and heating of the mixture is continued until the reaction is complete. The hot mixture is filtered over Hyflo and the filtrate is then evaporated. The residue is digested in a little hexane and then filtered, which gives 15 g (91.4%) of the title compound of m.p. 134°-136° C.

후처리

  1. customrises briefly to 31° C
  2. additionWhen the temperature has dropped again to 25° C.
  3. temperaturethe mixture is heated
  4. temperaturerefluxed overnight
  5. temperatureheating of the mixture
  6. filtrationThe hot mixture is filtered over Hyflo
  7. customthe filtrate is then evaporated
  8. filtrationfiltered

출처 및 근거

ORD 기록
ord-e7c17657d5874034be389a4126755d23
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05260423

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