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HRID888674

反应详情

EQUATION

反应方程式

HRID 888674 的结构方程式

REACTANTS

反应物

3
结构：II
HCID807

Iodine

I2

结构：O=S([O-])([O-])=S.[Na+].[Na+]
HCID24477

Sodium thiosulfate

Na2O3S2

结构：CC(C)[C@H]1NC(=O)[C@@H](CSC(c2ccccc2)(c2ccccc2)c2ccccc2)NC(=O)[C@@H](Cc2ccccc2)CC(=O)N[C@@H](/C=C/CCSC(c2ccccc2)(c2ccccc2)c2ccccc2)OOC(=O)C[C@@H]1O
HCID86639714

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)[C@H]1NC(=O)[C@H]2CSSCC/C=C/[C@H](NC(=O)C[C@H](Cc3ccccc3)C(=O)N2)OOC(=O)C[C@@H]1O
HCID86639716

未命名化合物

收率 68%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO.ClCCl
溶剂HCID21226129

未命名化合物

2 次

PROCEDURE

实验过程

To a solution of iodine (198.4 mg, 0.78 mmol) in CH2Cl2/MeOH (9:1, 272 mL) was added dropwise a solution of 6A (79.4 mg, 0.08 mmol) in CH2Cl2/MeOH (9:1) (134 mL) over 30 min, the reaction mixture was then allowed to stir for a further 30 min after which time sodium thiosulfate (88 mL, 0.05 M) was added. The layers were separated and the product was extracted with CH2Cl2 (3×45 ml) dried (MgSO4) and the solvent was removed in vacuo. Purification was then carried out by column chromatography on silica gel (eluent 3:97 MeOH/CH2Cl2) which gave 7A (30 mg, mmol, 68%) as a white solid: Rf 0.19 CH2Cl2/MeOH (97:3); [α]26D=−83.7 (c 0.38, MeOH).

WORKUP

后处理

  1. additionwas added
  2. customThe layers were separated
  3. extractionthe product was extracted with CH2Cl2 (3×45 ml)
  4. dry with materialdried (MgSO4)
  5. customthe solvent was removed in vacuo
  6. customPurification