O-Xylene → 7-Thia-2,4,5-triazatricyclo(6.4.0.0,2,6)dodeca-1(12),3,5,8,10-pentaene

HRID 461845

반응식

HRID 461845 반응식
[NH:1]([C:3]1[S:4][C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1)[NH2:2].[CH:12]([O-])([O-])OCC.C1(C)C(C)=CC=CC=1>C(O)C>[N:1]1[N:2]=[CH:12][N:7]2[C:6]3[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=3[S:4][C:3]=12

참가 물질

5

반응물 3

HCID 7237O-XyleneHCID 119882-Benzothiazolinone, hydrazoneHCID 53630039Ethylorthoformate

생성물 1

HCID 2545687-Thia-2,4,5-triazatricyclo(6.4.0.0,2,6)dodeca-1(12),3,5,8,10-pentaene

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
105 °C

실험 절차

2-Hydrazinobenzothiazole (125 grams; 0.76 mole), ethyl orthoformate (112.4 grams, 0.76 mole), and 2 liters of xylene were heated together with stirring in a three-necked 5-liter flask. An 8-inch column with a condenser was placed in one neck. The reaction was heated to 105° C. and soon all the solid had gone into solution and the solution turned red. Ethanol began to distill from the reaction and about 125 milliliters of it was collected before the reaction was stopped and allowed to cool to room temperature. The yellow precipitate was collected and triturated with diethyl ether. The s-triazolo(3,4-b)benzothiazole product thus obtained was recrystallized from chloroform, m.p. 174.5°-7° C.

후처리

  1. customAn 8-inch column with a condenser was placed in one neck
  2. distillationto distill from the reaction and about 125 milliliters of it
  3. customwas collected before the reaction
  4. temperatureto cool to room temperature
  5. customThe yellow precipitate was collected
  6. customtriturated with diethyl ether

출처 및 근거

ORD 기록
ord-32565a56ae524afb9e1860d1f9acf36f
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04064261

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