HCID 20232011、化合物 → HCID 15586410、化合物

HRID 2290363ノート

反応式

HRID 2290363 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([NH:14][NH2:15])=[N:10][C:9]=2[CH3:16])=[CH:4][CH:3]=1.ICS[C:20]1[NH:21][CH2:22][CH2:23][N:24]=1>C(O)CCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:13]=[N:12][C:11]([NH:14][NH:15][C:20]3[NH:24][CH2:23][CH2:22][N:21]=3)=[N:10][C:9]=2[CH3:16])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 20232011HCID 20232011、化合物HCID 20232073HCID 20232073、化合物

生成物 1

HCID 15586410HCID 15586410、化合物収率 17%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of 6-(4-chlorophenyl)-3-hydrazino-5-methyl-1,2,4-triazine (7 g), 2-iodomethylthio-2-imidazoline (8.11 g) and n-butanol (50 ml) was refluxed for 3 hours with stirring. After cooling, the mixture was evaporated under reduced pressure and the residue was dissolved in 1N hydrochloric acid. The solution was washed with ethyl acetate and made alkaline with an aqueous solution of potassium carbonate. The resultant precipitates were collected by filtration, washed with water, dried and recrystallized from methanol and then from ethanol to give dark red crystals of 6-(4-chlorophenyl)-3-[2-(2-imidazolin-2-yl)hydrazino]-5-methyl-1,2,4-triazine (1.53 g), m.p. 230°~231° C. (decomp.).

後処理

  1. temperaturewas refluxed for 3 hours
  2. temperatureAfter cooling
  3. customthe mixture was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in 1N hydrochloric acid
  5. washThe solution was washed with ethyl acetate
  6. customThe resultant precipitates
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customdried
  10. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-62ab3297fbc64afdbb932da8de2854f1
出典データセット
uspto-grants-1986_10
特許番号
US04616014

反応ノート

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