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HRID851674

反应详情

EQUATION

反应方程式

HRID 851674 的结构方程式

REACTANTS

反应物

1
结构：CC(=O)OC[C@H]1O[C@H](SCCC(=O)NCCCC[C@H](NC(=O)[C@H](CCCCNC(=O)CCS[C@H]2O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]2OC(C)=O)NC(=O)CCS[C@H]2O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]2OC(C)=O)C(=O)O)[C@@H](OC(C)=O)[C@@H](OC(C)=O)[C@@H]1OC(C)=O.N#N
HCID86738897

未命名化合物

PRODUCTS

生成物

1
结构：N#N.O=C(CCS[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@@H]1O)NCCCC[C@H](NC(=O)[C@H](CCCCNC(=O)CCS[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@@H]1O)NC(=O)CCS[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@@H]1O)C(=O)O
HCID86738896

未命名化合物

收率 90%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCN(CC)CC.CO.O
溶剂HCID23434731

未命名化合物

PROCEDURE

实验过程

A solution of 4 (2.0 g) in methanol-water-triethylamine 5:4:1 (v/v/v, 20 ml) is kept overnight at room temperature, and evaporated in vacuo to a residue that is put on a column of silica gel and eluted with chloroform-methanol-water 60:40:10 (v/v/v). The desired fractions are combined and evaporated to dryness. A solution of this compound in water (15 ml) is lyophilized to give 5 (1.2 g, 90%): mp 95°-100° C.; [α]D27 +115±0.9° (c 1.1, H2O); NMR (D2O) δ: 5.37 (s, 1H, H-1), 5.34 (s, 2H, H-1), 4.36, 4.19 (q,q, α-CH), 3.24 (m, ε-CH2), 2.95 (m, SCH2), 2.71 (t, 2H), 2.61 (t, 4H) (SCH2CH2), 1.33-1.92 (CCH2CH2CH2C).

WORKUP

后处理

  1. customevaporated in vacuo to a residue that
  2. washeluted with chloroform-methanol-water 60:40:10 (v/v/v)
  3. customevaporated to dryness