Sodium Bicarbonate → 1,3-Diazaazulene

HRID 359925

반응식

HRID 359925 반응식
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

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 178527782HCID 178527782, 화합물

생성물 1

HCID 6380091,3-Diazaazulene

시약·촉매·용매 1

HCID 944Nitric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-806c2780e8554cf79948790b40336afd
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05003077

연결된 노트

불러오는 중…