Methanol → HCID 86744075、化合物

HRID 2165254ノート

反応式

HRID 2165254 の反応式
[NH2:1][C@H:2]1[CH2:6][CH2:5][NH:4][CH2:3]1.[C:7]([OH:16])(=[O:15])[C@@H:8]([C@H:10]([C:12]([OH:14])=[O:13])[OH:11])[OH:9].CO>O>[C:12]([C@@H:10]([C@H:8]([C:7]([OH:16])=[O:15])[OH:9])[OH:11])([OH:14])=[O:13].[NH2:1][C@H:2]1[CH2:6][CH2:5][NH:4][CH2:3]1

参加物

5

反応物 3

HCID 887MethanolHCID 444305L-Tartaric acidHCID 1519351(3S)-(-)-3-Aminopyrrolidine

生成物 1

HCID 86744075HCID 86744075、化合物収率 38.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The above crude (3S)-3-aminopyrrolidine (200 mg) and L(+)-tartaric acid (348 mg) are dissolved in water (2 ml), and thereto is added methanol (10 ml), and the mixture is allowed to stand at room temperature for one hour to precipitate an oily substance. The superfluid is removed by decantation, and the oily substance is dissolved in a mixed solvent of methanol-water (1:1) with heating, and then the mixture is cooled, and the precipitated impurities are removed by filtration. The filtrate is concentrated to dryness, and the residue is recrystallized from a mixed solvent of methanol-water (2:3) to give (3S)-3-aminopyrrolidine L(+)-tartrate (210 mg).

後処理

  1. customto precipitate an oily substance
  2. customThe superfluid is removed by decantation
  3. dissolutionthe oily substance is dissolved in a mixed solvent of methanol-water (1:1)
  4. temperaturewith heating
  5. temperaturethe mixture is cooled
  6. customthe precipitated impurities are removed by filtration
  7. concentrationThe filtrate is concentrated to dryness
  8. customthe residue is recrystallized from a mixed solvent of methanol-water (2:3)

出典と根拠

ORDレコード
ord-7e9bee35351c4f7a9eabdcf6ad8a6a43
出典データセット
uspto-grants-1990_07
特許番号
US04939256

反応ノート

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