Sodium Bicarbonate → 1,3-Diazaazulene

HRID 1194295

반응식

HRID 1194295 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

With reference to Journal of the American Chemical Society, vol. 76, pages 3352 and 3353 (1954), 23 g of 2-mercaptocycloheptimidazole as synthesized in Synthetic example 1 (b) was added to 210 ml of 10% nitric acid, and stirred with heating to the inner temperature of 80° to 90° C. for one hour. The reaction solution was neutralized with sodium bicarbonate and extracted with chloroform (250 ml×2). The chloroform layer was dried over anhydrous sodium sulfate and concentrated to 50 ml under reduced pressure, and then 200 ml of hexane was added. Deposited crystals were collected by filtration and dried.

후처리

  1. temperaturewith heating to the inner temperature of 80° to 90° C. for one hour
  2. extractionextracted with chloroform (250 ml×2)
  3. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated to 50 ml under reduced pressure
  5. addition200 ml of hexane was added
  6. filtrationDeposited crystals were collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-25bb50e9cc084d5995ba5bdafc42784e
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04814265

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