Hydrochloric Acid → HCID 178494713, 화합물

HRID 1700735노트

반응식

HRID 1700735 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[CH2:16][C:15]2[NH:14][N:13]=[C:12]([CH2:17][O:18][CH3:19])[C:11]=2[C:10](=O)[CH2:9]1.[C:21]([NH:24][NH2:25])([NH2:23])=[NH:22].Cl.Cl.O>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[CH2:16][C:15]2[NH:14][N:13]=[C:12]([CH2:17][O:18][CH3:19])[C:11]=2[C:10](=[N:25][NH:24][C:21]([NH2:23])=[NH:22])[CH2:9]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 183176226-(2-Chlorophenyl)-3-methoxymethyl-4,5,6,7-tetrahydroindazol-4-oneHCID 178418668HCID 178418668, 화합물

생성물 1

HCID 178494713HCID 178494713, 화합물수율 91%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 6-(2-chlorophenyl)-3-methoxymethyl-4,5,6,7-tetrahydroindazol-4-one (0.1 g), aminoguanidine hydrochloride (0.046 g), concentrated hydrochloric acid (0.086 ml), water (0.086 ml) and ethanol (10 ml) was refluxed for 5 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added sodium hydrogen carbonate solution to make the solution alkaline. The mixture was extracted with ethyl acetate, and the organic layer was washed with water and concentrated under reduced pressure. The residue was dissolved in 1N hydrochloric acid (1ml), and the solution was concentrated. The resulting crystals were recrystallized from ethanol-ethyl acetate to give 6-(2-chlorophenyl)-4-guanidinoimino-3-methoxymethyl-4,5,6,7-tetrahydroindazole hydrochloride (Compound 148) (0.06 g) as colorless crystals.

후처리

  1. temperaturewas refluxed for 5 hours
  2. customUnder reduced pressure, the solvent was evaporated
  3. additionto the residue was added sodium hydrogen carbonate solution
  4. extractionThe mixture was extracted with ethyl acetate
  5. washthe organic layer was washed with water
  6. concentrationconcentrated under reduced pressure
  7. dissolutionThe residue was dissolved in 1N hydrochloric acid (1ml)
  8. concentrationthe solution was concentrated
  9. customThe resulting crystals were recrystallized from ethanol-ethyl acetate

출처 및 근거

ORD 기록
ord-b27811c90a39471daaf3c9691ae743c6
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06350749B1

반응 노트

불러오는 중…