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

HRID 257132

反応式

HRID 257132 の反応式
[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

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒2 回HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e7c17657d5874034be389a4126755d23
出典データセット
uspto-grants-1993_11
特許番号
US05260423

関連ノート

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