Hydrazine hydrate (1:1) → 3-Hydrazino-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide

HRID 481964

반응식

HRID 481964 반응식
O.CS[C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1.O.[NH2:17][NH2:18]>CO>[NH:17]([C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1)[NH2:18]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 190647513-Methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate

생성물 1

HCID 101305633-Hydrazino-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
70 °C

실험 절차

3-Methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate (1.0 g) was added to hydrazine hydrate (0.8 ml) and the mixture was heated to 70° C. for 30 min. After cooling, the reaction mixture was supplemented with methanol (10 ml) and the solvents were removed by distillation under reduced pressure. The residue was dissolved in NaOH 2M (20 ml), treated with charcoal, filtered, and the filtrate was adjusted to pH 6-7 with HCl 1M. The precipitate so obtained was collected by filtration, washed with water an dried (yield: 0.8 g); m.p. 290°-292° C. (Compound 1).

후처리

  1. temperatureAfter cooling
  2. customthe solvents were removed by distillation under reduced pressure
  3. dissolutionThe residue was dissolved in NaOH 2M (20 ml)
  4. additiontreated with charcoal
  5. filtrationfiltered
  6. customThe precipitate so obtained
  7. filtrationwas collected by filtration
  8. washwashed with water
  9. customan dried (yield: 0.8 g)

출처 및 근거

ORD 기록
ord-ee90a9060b474eaebf3e5432d679e53d
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05792764

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