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

HRID 481964

反応式

HRID 481964 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-ee90a9060b474eaebf3e5432d679e53d
出典データセット
uspto-grants-1998_08
特許番号
US05792764

関連ノート

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