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Hydrazine hydrate (1:1) → 4-[2-(2,2,2-Trifluoroethyl)guanidino]-2-(2-aminoethylthio)pyrimidine

HRID 1902302
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반응식

HRID 1902302 반응식
[F:1][C:2]([F:29])([F:28])[CH2:3][N:4]=[C:5]([NH2:27])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([S:13][CH2:14][CH2:15][N:16]2C(=O)C3=CC=CC=C3C2=O)[N:8]=1.O.NN>C(O)C>[F:29][C:2]([F:1])([F:28])[CH2:3][N:4]=[C:5]([NH2:27])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([S:13][CH2:14][CH2:15][NH2:16])[N:8]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 212987304-[2-(2,2,2-Trifluoroethyl)guanidino]-2-(2-phthalimidoethylthio)pyrimidine

생성물 1

HCID 212988314-[2-(2,2,2-Trifluoroethyl)guanidino]-2-(2-aminoethylthio)pyrimidine수율 60.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 4-[2-(2,2,2-trifluoroethyl)-guanidino]-2-(2-phthalimidoethylthio)pyrimidine (0.6 g.) ethanol (20 ml.) and 99% hydrazine hydrate (0.5 ml.) was heated under reflux for 1 hour and then evaporated to dryness. The residue was stirred with N hydrochloric acid and the mixture filtered. The filtrate was basified with 17 N NaOH and the mixture extracted three times with ether. The combined ether extracts were dried and then evaporated to dryness to give 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-(2-aminoethylthio)pyrimidine (0.25 g.) which was used without further purification.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. customevaporated to dryness
  4. filtrationthe mixture filtered
  5. extractionthe mixture extracted three times with ether
  6. dry with materialThe combined ether extracts were dried
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-4b6425fb03ff4abfbb47140fb23d112a
출처 데이터셋
uspto-grants-1982_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04362728

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