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

HRID 461845

反応式

HRID 461845 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
105 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32565a56ae524afb9e1860d1f9acf36f
出典データセット
uspto-grants-1977_12
特許番号
US04064261

関連ノート

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