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HRID266024

反应详情

EQUATION

反应方程式

HRID 266024 的结构方程式

REACTANTS

反应物

4
结构：CCN(CC)CC
HCID8471

Triethylamine

C6H15N

结构：C=CCCC(=O)O
HCID61138

4-Pentenoic acid

C5H8O2

结构：CC(C)COC(=O)Cl
HCID62365

Isobutyl chloroformate

C5H9ClO2

结构：COC(=O)CC[C@@H](C)[C@H]1CC[C@H]2[C@@H]3[C@H](O)C[C@@H]4C[C@@H](N)CC[C@]4(C)[C@H]3C[C@H](O)[C@]12C
HCID10364902

未命名化合物

PRODUCTS

生成物

1
结构：C=CCCC(=O)N[C@H]1CC[C@@]2(C)[C@@H](C1)C[C@@H](O)[C@@H]1[C@@H]2C[C@H](O)[C@]2(C)[C@@H]([C@H](C)CCC(=O)OC)CC[C@@H]12
HCID54437505

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

2 次

PROCEDURE

实验过程

A solution of 4-pentenoic acid (marketed product) and triethylamine in THF was added drop by drop, under nitrogen and at 5° C., to isobutyl chloroformate and subsequently with a solution of (3β,5β,7α,12α)-3-amino-7,12-dihydroxy-cholan-24-oic acid methyl ester (prepared according to the procedure described in EXAMPLE 5) in THF. When the reaction was over, solvent was evaporated and the residue was taken up with H2O and AcOEt. The organic phase was separated, washed with H2O, dried over Na2SO4 and evaporated under reduced pressure. The residue was purified by flash chromatography to obtain the desired product.

WORKUP

后处理

  1. customwas evaporated
  2. customThe organic phase was separated
  3. washwashed with H2O
  4. dry with materialdried over Na2SO4
  5. customevaporated under reduced pressure
  6. customThe residue was purified by flash chromatography