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HRID724553

反应详情

EQUATION

反应方程式

HRID 724553 的结构方程式

REACTANTS

反应物

3
结构：c1ccncc1
HCID1049

Pyridine

C5H5N

结构：CSCCl
HCID16916

Chlorodimethyl sulfide

C2H5ClS

结构：CC#C[C@@]1(O)CC[C@H]2[C@@H]3CCC4=CC(=O)CCC4=C3[C@@H](c3ccc(N(C)CCO[C@H]4CC[C@@]5(C)[C@@H](C4)C[C@@H](O)[C@@H]4[C@@H]5C[C@H](O)[C@]5(C)[C@@H]([C@H](C)CCC(=O)OC)CC[C@@H]45)cc3)C[C@@]21C
HCID131726114

未命名化合物

PRODUCTS

生成物

1
结构：CC#C[C@@]1(O)CC[C@H]2[C@@H]3CCC4=CC(=O)CCC4=C3[C@@H](c3ccc(N(C)CCO[C@H]4CC[C@@]5(C)[C@@H](C4)C[C@@H](OCSC)[C@@H]4[C@@H]5C[C@H](O)[C@]5(C)[C@@H]([C@H](C)CC(C)C(=O)O)CC[C@@H]45)cc3)C[C@@]21C
HCID131726118

未命名化合物

PROCEDURE

实验过程

The compound of Example 1I is dissolved in pyridine and cooled in an ice bath; methylthiomethyl chloride (1.2 eq) is added, and the mixture is warmed to ambient temperature, then heated to 90° C. overnight. The solvents are removed in vacuo; the residue is partitioned between aqueous phosphoric acid (1N) and ethyl acetate. The organic extract is washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo. The crude material is purified by column chromatography.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. temperatureheated to 90° C. overnight
  3. customThe solvents are removed in vacuo
  4. customthe residue is partitioned between aqueous phosphoric acid (1N) and ethyl acetate
  5. extractionThe organic extract
  6. washis washed with brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe crude material is purified by column chromatography