Hydrazine Sulfate → HCID 178485006、化合物

HRID 258743

反応式

HRID 258743 の反応式
[ClH:1].Cl.O[NH:4][C:5]([NH:17][CH3:18])=[N:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16].S(O)(O)(=O)=O.[NH2:24]N.C(=O)([O-])O.[K+]>CN(C)C=O>[ClH:1].[ClH:1].[NH2:24][NH:4][C:5]([NH:17][CH3:18])=[N:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16]

参加物

5

反応物 3

HCID 24842Hydrazine SulfateHCID 516893Potassium BicarbonateHCID 178485010HCID 178485010、化合物

生成物 1

HCID 178485006HCID 178485006、化合物収率 46.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

A mixture of the isothiourea dihydrochloride from Example 1 (i) (8.3 g), hydrazine sulphate (4.1 g), potassium hydrogen carbonate (12.5 g) and anhydrous dimethyl formamide (100 ml) was stirred at 90° C. for 3 hours. Following cooling and filtration from inorganic material, the filtrate containing the free base was treated with ethanolic hydrogen chloride. The residue was then triturated with isopropanol to give a solid which was recrystallised from aqueous isopropanol to give the title compound (1.94 g), m.p. 234°-235°.

後処理

  1. temperatureFollowing cooling
  2. filtrationfiltration from inorganic material
  3. additionthe filtrate containing the free base
  4. additionwas treated with ethanolic hydrogen chloride
  5. customThe residue was then triturated with isopropanol
  6. customto give a solid which
  7. customwas recrystallised from aqueous isopropanol

出典と根拠

ORDレコード
ord-2179ab7713b242788365fa0853126697
出典データセット
uspto-grants-1977_07
特許番号
US04034101

関連ノート

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