N-Methylethylenediamine → 1-Methyl-2(1,3-dimethyl-5-pyrazolyl) amino-2-imidazoline

HRID 903086ノート

反応式

HRID 903086 の反応式
I.[CH3:2][N:3]1[C:7]([NH:8][C:9](=N)SC)=[CH:6][C:5]([CH3:13])=[N:4]1.[CH3:14][NH:15][CH2:16][CH2:17][NH2:18]>C(Cl)Cl>[CH3:14][N:15]1[CH2:16][CH2:17][N:18]=[C:9]1[NH:8][C:7]1[N:3]([CH3:2])[N:4]=[C:5]([CH3:13])[CH:6]=1

参加物

4

実験手順

N(1,3-Dimethyl-5-pyrazolyl)-5-methyl isothiourea hydroiodide (Example XXV) (20.0 g) and 11.5 g. -N-methyl ethylenediamine were heated to 120° for 30 minutes and to 160° for 1 hour. After cooling, methylene chloride was added and the solid which formed was filtered and discarded. The methylene chloride solution was shaken with 15% KOH solution, dried over potassium carbonate, concentrated and the residue crystallized from acetonitrile to get 10.16 g. product, mp. 128°-130°.

後処理

  1. temperatureAfter cooling
  2. customthe solid which formed
  3. filtrationwas filtered
  4. dry with materialdried over potassium carbonate
  5. concentrationconcentrated
  6. customthe residue crystallized from acetonitrile
  7. customto get 10.16 g

出典と根拠

ORDレコード
ord-f62175181ee54a6f90e94942f77e4652
出典データセット
uspto-grants-1980_10
特許番号
US04226773

反応ノート

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