Guanidine → HCID 178432057、化合物

HRID 1384291ノート

反応式

HRID 1384291 の反応式
[NH2:1][C:2]([NH2:4])=[NH:3].[CH3:5][C:6]1[N:11]=[C:10]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:9]2=[CH:8][C:7]=1[C:17](OCC)=[O:18]>CC(O)C>[CH3:5][C:6]1[N:11]=[C:10]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:9]2=[CH:8][C:7]=1[C:17]([NH:3][C:2]([NH2:4])=[NH:1])=[O:18]

参加物

4

反応物 2

HCID 3520GuanidineHCID 21186750HCID 21186750、化合物

生成物 1

HCID 178432057HCID 178432057、化合物収率 31.2%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

In an atmosphere of argon, metallic sodium (325.2 mg, 0.014 g atom) was dissolved in anhydrous methanol (20.0 ml) at room temperature, and the solution was mixed with guanidine hydrochloride (1.35 g, 14.1 mmol) at 0° C. After 1 hour of stirring at room temperature, the thus precipitated sodium chloride was removed by filtration using a glass filter and the resulting filtrate was evaporated under reduced pressure to obtain free guanidine. Guanidine and ethyl 2-methyl-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carboxylate (500.0 mg, 2.02 mmol) were suspended in 2-propanol (12.0 ml) and heated under reflux for 18 hours. After cooling, the solvent was evaporated under reduced pressure, and the resulting residue was mixed with water and extracted with ethyl acetate. The thus obtained organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure and then the thus formed crystals were washed with ether to obtain the title compound (165.1 mg, 31.2%) as white powder.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 18 hours
  3. temperatureAfter cooling
  4. customthe solvent was evaporated under reduced pressure
  5. additionthe resulting residue was mixed with water
  6. extractionextracted with ethyl acetate
  7. dry with materialThe thus obtained organic layer was dried over anhydrous sodium sulfate
  8. customthe solvent was evaporated under reduced pressure
  9. washthe thus formed crystals were washed with ether

出典と根拠

ORDレコード
ord-4f2725909eaf4aeb80b659231a921b11
出典データセット
uspto-grants-2001_07
特許番号
US06258829B1

反応ノート

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