Cyanogen Bromide → Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-

HRID 1714702

反応式

HRID 1714702 の反応式
N#[C:2]Br.CC(N[C@H]1[C@H](O)O[C@H]([O:15][S:16]([OH:19])(=O)=[O:17])[C@H](O)[C@@H]1O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O)=O.[OH-].[Na+].C1C(N)=CC2C(O[C:46]3([C:56]4C=CC(O)=CC=4[O:54][C:48]4[CH:49]=[C:50](O)[CH:51]=[CH:52][C:47]3=4)[C:38]=2C=1)=O>B([O-])([O-])[O-].[Na+].[Na+].[Na+].O>[CH3:56][C:46]1([CH3:38])[C:47]2([CH2:2][S:16]([OH:19])(=[O:17])=[O:15])[C:48]([CH2:49][CH:50]1[CH2:51][CH2:52]2)=[O:54]

参加物

7

反応物 4

HCID 10476Cyanogen BromideHCID 14798Sodium HydroxideHCID 24766Chondroitin Sulfate3 回HCID 768455-Aminofluorescein

生成物 1

HCID 18462Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 159383boric acid, sodium salt溶媒2 回

実験手順

20 mg cyanogen bromide (CNBr) dissolved in 200 μl deionized water were added to 1 ml of 30 mg/ml chondroitin 4-sulfate (CSA). The pH was adjusted to pH 11 by addition of 5 M NaOH. Activated CSA is applied to a PD-10 column and eluded with 200 mM sodium borate buffer, pH 8.0. CSA fractions were directly dropped into 400 μl of 10 mg/ml fluoresceinamine in 200 mM sodium borate buffer, pH 8.0. The mixture was kept overnight at 4° C. for the coupling reaction. Subsequently, the mixture was concentrated to 1 ml using a SpeedVac concentrator and purified on a PD-10 column and eluded by 50 mM sodium acetate buffer, pH 5.5. Fluoresceinamine-labeled CSA (FL-CSA) fractions were collected and their concentration was determined using the Blyscan glycosaminoglycan assay kit (Biocolor Ltd., Newtown Abbey, Northern Ireland).

後処理

  1. customThe mixture was kept overnight at 4° C. for the coupling reaction
  2. concentrationSubsequently, the mixture was concentrated to 1 ml
  3. custompurified on a PD-10 column
  4. customwere collected
  5. concentrationtheir concentration

出典と根拠

ORDレコード
ord-89998e36e64f4c26a795147bddb96aed
出典データセット
uspto-grants-2010_09
特許番号
US07799326B2

関連ノート

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