Sodium Bicarbonate → 1,3-Diazaazulene

HRID 359925

反応式

HRID 359925 の反応式
S[C:2]1[N:3]=[C:4]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=[C:5]2[N:6]=1.C(=O)([O-])O.[Na+]>[N+]([O-])(O)=O>[N:3]1[C:4]2=[CH:11][CH:10]=[CH:9][CH:8]=[CH:7][C:5]2=[N:6][CH:2]=1

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 178527782HCID 178527782、化合物

生成物 1

HCID 6380091,3-Diazaazulene

試薬・触媒・溶媒 1

HCID 944Nitric Acid溶媒

実験手順

In accordance with the method described in Journal of the Americal Chemical Society, Vol. 76, pages 3352 and 3353 (1954), 23 g of 2-mercaptocycloheptimidazole, as obtained in Example 1-(b), was added to 210 ml of 10% nitric acid and everything was stirred under heating at an internal temperature of from 80° to 90° C. for 1 hour. Sodium hydrogencarbonate was added to the reaction solution so as to neutralize the solution, and this was extracted with chloroform (250 ml×2). The chloroform layer was dried with anhydrous sodium sulfate, and then the solvent was evaporated off until the amount of the chloroform solution became 50 ml. Next, 200 ml of hexane was added thereto. The crystals precipitated were separated by filtration and dried.

後処理

  1. temperatureunder heating at an internal temperature of from 80° to 90° C. for 1 hour
  2. extractionthis was extracted with chloroform (250 ml×2)
  3. dry with materialThe chloroform layer was dried with anhydrous sodium sulfate
  4. customthe solvent was evaporated off until the amount of the chloroform solution
  5. additionNext, 200 ml of hexane was added
  6. customThe crystals precipitated
  7. customwere separated by filtration
  8. customdried

出典と根拠

ORDレコード
ord-806c2780e8554cf79948790b40336afd
出典データセット
uspto-grants-1991_03
特許番号
US05003077

関連ノート

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