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Sulfuric Acid → Xylostasin

HRID 437262
ノート
印刷プレビュー

反応式

HRID 437262 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 1 N sulfuric acid. The resulting precipitate of barium sulfate is removed off by centrifuge. The supernatant fluid is run onto a colume of 300 parts by volume of cation exchange resin (Amberlite CG-50(NH4 +-form) (Rohm and Haas Co.)). The colume is washed with water and eluted with 0.2 N 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 colume is washed with water
  5. washeluted with 0.2 N 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-7e17ae40e3274a2dabdb7be6ec73ee50
出典データセット
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04029883

反応ノート

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