[1]benzothiolo[3,2-d]triazin-4-ylhydrazine → HCID 12269874, 화합물

HRID 328675노트

반응식

HRID 328675 반응식
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

참가 물질

3

반응물 1

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

생성물 1

HCID 12269874HCID 12269874, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7489a842ce2743f1ba71f31bdd789d2c
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018768

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