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Sulfuric Acid → Xylostasin

HRID 329309
ノート
印刷プレビュー

反応式

HRID 329309 の反応式
S(=O)(=O)(O)O.[CH2:6]1[C@@H:11]([NH:12]C([C@@H](O)CCN)=O)[C@H:10]([OH:20])[C@@H:9]([O:21][C@@H:22]2[O:26][C@H:25]([CH2:27][OH:28])[C@H:24]([OH:29])[C@H:23]2[OH:30])[C@H:8]([O:31][C@H:32]2[O:37][C@H:36]([CH2:38][NH2:39])[C@@H:35]([OH:40])[C@H:34]([OH:41])[C@H:33]2[NH2:42])[C@H:7]1[NH2:43]>[OH-].[Ba+2].[OH-]>[CH2:6]1[C@H:7]([NH2:43])[C@@H:8]([O:31][C@H:32]2[O:37][C@H:36]([CH2:38][NH2:39])[C@@H:35]([OH:40])[C@H:34]([OH:41])[C@H:33]2[NH2:42])[C@H:9]([O:21][C@@H:22]2[O:26][C@H:25]([CH2:27][OH:28])[C@H:24]([OH:29])[C@H:23]2[OH:30])[C@@H:10]([OH:20])[C@@H:11]1[NH2:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 12302171Butirosin A

生成物 1

HCID 73079Xylostasin

試薬・触媒・溶媒 1

HCID 6093286Barium hydroxide溶媒

実験手順

In 250 parts by volume of an 0.5N aqueous solution of barium hydroxide is dissolved 5.0 parts of butirosin A. The solution is refluxed for 2 hours and then cooled. The solution is neutralized with 1N sulfuric acid. The resulting precipitate of barium sulfate is removed off by centrifuge. The supernatant fluid is run onto a column of 300 parts by volume of cation exchange resin [Amberlite CG-50 (NH4+ -form) (Rohm and Haas Co.)]. The column is washed with water and eluted with 0.2N aqueous ammonia. Fractions containing xylostasin which is detected by thin layer chromatography are pooled and concentrated under reduced pressure to dryness and lyophilized, whereby 3.8 parts of xylostasin as white powders are obtained.

後処理

  1. temperatureThe solution is refluxed for 2 hours
  2. temperaturecooled
  3. customThe resulting precipitate of barium sulfate is removed off by centrifuge
  4. washThe column is washed with water
  5. washeluted with 0.2N aqueous ammonia
  6. additionFractions containing xylostasin which
  7. concentrationconcentrated under reduced pressure to dryness

出典と根拠

ORDレコード
ord-f362b8e0f91c4a4ba65af306cb47c3c9
出典データセット
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04020269

反応ノート

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