Hydrochloric Acid → HCID 178502873, 화합물

HRID 67909

반응식

HRID 67909 반응식
C[CH:2]([NH2:15])C(O)C1C=C(OC)C=CC=1OC.Cl.[OH-:17].[K+].CSC(=[N:24][C:25]#[N:26])SC.[CH3:27][C:28]1[N:29]=[CH:30][NH:31][C:32]=1[CH2:33][S:34][CH2:35][CH2:36][NH2:37].[CH3:38]O>O>[C:25]([NH:24][C:2]([NH:15][O:17][CH3:38])=[N:37][CH2:36][CH2:35][S:34][CH2:33][C:32]1[NH:31][CH:30]=[N:29][C:28]=1[CH3:27])#[N:26]

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 887Methanol3회HCID 6082MethoxamineHCID 14797Potassium HydroxideHCID 66289Dimethyl N-cyanodithioiminocarbonateHCID 178433288HCID 178433288, 화합물

생성물 1

HCID 178502873HCID 178502873, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of methoxamine (7.0 g), prepared from the hydrochloride and potassium hydroxide in methanol (50 ml) and water (10 ml) was added to a solution of dimethylcyanodithioimidocarbonate (7.3 g) in methanol (40 ml) and stirred at room temperature for 60 hours. A solution of 4-methyl-5-[(2-aminoethyl)thiomethyl]imidazole (8.6 g) in methanol (30 ml) was added and the resulting solution was heated under reflux for 18 hours. Concentration followed by chromatographic purification on a column of silica gel with chloroform-methanol (10:1) as eluant and final recrystallisation from acetonitrile afforded the title compounds m.p. 155°-6°

후처리

  1. temperaturethe resulting solution was heated
  2. temperatureunder reflux for 18 hours
  3. concentrationConcentration
  4. customfollowed by chromatographic purification on a column of silica gel with chloroform-methanol (10:1) as eluant
  5. customfinal recrystallisation from acetonitrile

출처 및 근거

ORD 기록
ord-db29a31065ea4a9bba1787ca9a1d4937
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04347250

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