HCID 20232011, 화합물 → HCID 15586410, 화합물

HRID 2290363노트

반응식

HRID 2290363 반응식
[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

참가 물질

4

반응물 2

HCID 20232011HCID 20232011, 화합물HCID 20232073HCID 20232073, 화합물

생성물 1

HCID 15586410HCID 15586410, 화합물수율 17%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-62ab3297fbc64afdbb932da8de2854f1
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04616014

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