Hydrazine Sulfate → HCID 178485006, 화합물

HRID 258743

반응식

HRID 258743 반응식
[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]

참가 물질

5

반응물 3

HCID 24842Hydrazine SulfateHCID 516893Potassium BicarbonateHCID 178485010HCID 178485010, 화합물

생성물 1

HCID 178485006HCID 178485006, 화합물수율 46.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-2179ab7713b242788365fa0853126697
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04034101

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