Hydrochloric Acid → HCID 178494713、化合物

HRID 1700735ノート

反応式

HRID 1700735 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 178494713HCID 178494713、化合物収率 91%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b27811c90a39471daaf3c9691ae743c6
出典データセット
uspto-grants-2002_02
特許番号
US06350749B1

反応ノート

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