[1]benzothiolo[3,2-d]triazin-4-ylhydrazine → HCID 12269874、化合物

HRID 328675ノート

反応式

HRID 328675 の反応式
N([C:3]1[C:4]2[S:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[C:5]=2[N:6]=[N:7][N:8]=1)N>O>[N:6]1[C:5]2[C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[S:11][C:4]=2[CH:3]=[N:8][N:7]=1

参加物

3

反応物 1

HCID 323432[1]benzothiolo[3,2-d]triazin-4-ylhydrazine

生成物 1

HCID 12269874HCID 12269874、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 2.1 g. portion of the 4-hydrazino product of Example 5 was suspended in 130 ml. of water containing 5.4 g. of mercuric oxide and the mixture was stirred at reflux temperature for 4 hours. The mixture was then cooled and filtered, and the solids were triturated with hot ethyl acetate. After filtration, the filtrate was evaporated under vacuum. The residue was redissolved in ethyl acetate-hexane and was chromatographed over a silica gel column with 1:1 ethyl acetate-hexane as the eluant. The second product off the column was the desired product, which was recrystallized from denatured ethanol-water. The yield was 1.0 g. of [1]benzothieno[3,2-d]-v-triazine, m.p. 190°-191° C.

後処理

  1. temperatureat reflux temperature for 4 hours
  2. temperatureThe mixture was then cooled
  3. filtrationfiltered
  4. customthe solids were triturated with hot ethyl acetate
  5. filtrationAfter filtration
  6. customthe filtrate was evaporated under vacuum
  7. dissolutionThe residue was redissolved in ethyl acetate-hexane
  8. customwas chromatographed over a silica gel column with 1:1 ethyl acetate-hexane as the eluant
  9. customwas recrystallized from denatured ethanol-water

出典と根拠

ORDレコード
ord-7489a842ce2743f1ba71f31bdd789d2c
出典データセット
uspto-grants-1977_04
特許番号
US04018768

反応ノート

読み込み中…