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

HRID 364299
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반응식

HRID 364299 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 17N 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-0967d5554f364128a115a0dc11612059
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04604465

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