1,2-二氯乙烷 → 2-脱氧-D-葡萄糖

HRID 1353987

反应方程式

HRID 1353987 反应方程式
[OH-].[Na+].C1C(=O)N(O)C(=O)C1S([O-])(=O)=O.[Na+].C(Cl)CCl.Cl.[OH:21][CH:22]1[O:30][C@H:29]([CH2:31][OH:32])[C@@H:27]([OH:28])[C@H:25]([OH:26])[C@H:23]1N>O>[O:21]=[CH:22][CH2:23][C@H:25]([C@@H:27]([C@@H:29]([CH2:31][OH:32])[OH:30])[OH:28])[OH:26]

参与物

6

反应物 4

HCID 111,2-二氯乙烷HCID 14798二甲基对苯二胺二盐酸HCID 2723635D-氨基葡萄糖盐酸盐HCID 3520574N-羟基琥珀酰亚胺磺酸钠盐

产物 1

HCID 1082232-脱氧-D-葡萄糖

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

Sodium hydroxide (1N, 1 ml) was added to a stirred solution of EC (110 mg, 0.41 mmol) in water (5 ml). To this colorless solution, sulfo-NHS (241.6 mg, 1.12 mmol) and EDC (218.8 mg, 1.15 mmol) were added. D-Glucosamine hydrochloride salt (356.8 mg, 1.65 mmol) was then added. The mixture was stirred at room temperature for 24 hours. The mixture was dialyzed for 48 hours using Spectra/POR molecular porous membrane with cut-off at 500 (Spectrum Medical Industries Inc., Houston, Tex,). After dialysis, the product was frozen dried using lyophilizer (Labconco, Kansas City, Mo.). The product in the salt form weighed 568.8 mg. The synthetic scheme is shown in FIG. 59. The structure was confirmed by mass spectrometry (FIG. 60) and proton NMR (FIGS. 61 and 62). Radiochemical purity of 99mTc-EC-DG was 100% as determined by radio-TLC (FIG. 63) and HPLC (FIGS. 64 and 65) analysis.

后处理

  1. customThe mixture was dialyzed for 48 hours
  2. customAfter dialysis
  3. temperaturethe product was frozen
  4. customdried

来源与证据

ORD记录
ord-8150cb28e52e46609954cb80d3fdf66d
来源数据集
uspto-grants-2007_05
专利号
US07223380B2

关联笔记

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