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Hydrazine → 5-Chloro-6-hydrazinyl-3-nitropyrazin-2-amine

HRID 1903825
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HRID 1903825 반응식
[NH2:1][NH2:2].[Cl:3][C:4]1[N:5]=[C:6]([N+:12]([O-:14])=[O:13])[C:7]([NH2:11])=[N:8][C:9]=1Cl>C(O)C>[Cl:3][C:4]1[N:5]=[C:6]([N+:12]([O-:14])=[O:13])[C:7]([NH2:11])=[N:8][C:9]=1[NH:1][NH2:2]
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 130629765,6-Dichloro-3-nitropyrazin-2-amine

생성물 1

HCID 130629835-Chloro-6-hydrazinyl-3-nitropyrazin-2-amine수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 300 ml of ethanol was added 7.4 g (0.22 mole) of a 95% hydrazine solution. This solution was cooled to 10° and with stirring 20.9 g (0.1 mole) of 5,6-dichloro-3-nitropyrazinamine (l) was added portionwise. A dark precipitate formed immediately and the suspension was stirred for 1 hour at room temperature. The mixture was filtered and the resulting solid washed with ethanol, water, ethyl acetate, ethanol and air dried to afford 18.0 g (88%) of the desired hydrazine as a brown solid, m.p. 220°; ms:m/e 205. This solid was treated with acetone to form the isopropylidene derivative, m.p. 245°-246° (dec.).

후처리

  1. temperatureThis solution was cooled to 10°
  2. additionwas added portionwise
  3. customA dark precipitate formed immediately
  4. filtrationThe mixture was filtered
  5. washthe resulting solid washed with ethanol, water, ethyl acetate, ethanol and air
  6. customdried

출처 및 근거

ORD 기록
ord-aa7e1ebf2c7d46ec951c507123966cdb
출처 데이터셋
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04438266

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