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

HRID 34800
ノート
印刷プレビュー

反応式

HRID 34800 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c73bab9fc43b49d7ad23e75a2c95f975
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04762932

反応ノート

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