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HRID1105877

反应详情

EQUATION

反应方程式

HRID 1105877 的结构方程式

REACTANTS

反应物

3
结构：ClC(Cl)Cl
HCID6212

Chloroform

CHCl3

2 次

结构：[NH4+].[OH-]
HCID14923

Ammonium hydroxide

H5NO

结构：CC(=O)O[C@H]1[C@@H](OC(C)=O)[C@@H](CN2C(=O)c3ccccc3C2=O)O[C@@H](SCCCCCCO[C@H]2CC[C@@]3(C)C(=CC[C@H]4[C@@H]5CC[C@H]([C@H](C)CCCC(C)C)[C@@]5(C)CC[C@@H]43)C2)[C@@H]1OC(C)=O
HCID131712555

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)CCC[C@@H](C)[C@H]1CC[C@H]2[C@@H]3CC=C4C[C@@H](OCCCCCCS[C@@H]5O[C@H](CN)[C@H](O)[C@H](O)[C@H]5O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID131712556

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CO
溶剂HCID887

Methanol

CH4O

2 次

结构：CCCCN
溶剂HCID8007

Butylamine

C4H11N

PROCEDURE

实验过程

A suspension of 6-(5-cholesten-3β-yloxy)hexyl 2,3,4-tri-O-acetyl-6-deoxy-6-phthalimido-1-thio-β-D-galactopyranoside (710 mg.) in methanol (10 ml.) and n-butylamine (10 ml.) is heated under reflux for 16 hours. The solution is evaporated to a crystalline mass. Chloroform is added and the solid is filtered and washed with chloroform. The combined filtrates are evaporated to a syrup which is put on a column of silica gel and eluted with chloroform-methanol-ammonium hydroxide (80:20:2). The desired fractions are combined and evaporated to a syrup which is triturated with ethyl ether to give crystals (390 mg. 76%); Rf 0.28 (CHCl3 --MeOH--NH4OH, 80:20:2), [α]D27 -29.5° C. (C 1.05, chloroform), m.s.: m/e 665 (M+ +1).

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 16 hours
  3. customThe solution is evaporated to a crystalline mass
  4. additionChloroform is added
  5. filtrationthe solid is filtered
  6. washwashed with chloroform
  7. customThe combined filtrates are evaporated to a syrup which
  8. washeluted with chloroform-methanol-ammonium hydroxide (80:20:2)
  9. customevaporated to a syrup which
  10. customis triturated with ethyl ether
  11. customto give crystals (390 mg. 76%)