反应详情

In analogy with Example 1i), 1.4 g (2.79 mmol) of 5(S)-[1(S)-(Boc-amino)-2-phenylethyl]-3(R)-[(p-benzyloxyphenyl)methyl]dihydrofuran-2-(3H)-one in 45 ml of dimethoxyethane and 23 ml of water are hydrolysed with 11 ml of a 1M lithium hydroxide solution. The reaction mixture, which has been partially evaporated, is poured onto a mixture of ice, 137 ml of sat. NH4Cl solution, 11 ml of 10% citric acid solution and 56 ml of methylene chloride, and methanol is added until the precipitated solid dissolves. The aqueous phase is extracted with 2 portions of methylene chloride/methanol, approximately 10:1, and the organic phases are washed with saline, dried with Na2SO4 and evaporated: tRet (I)=24.0 min; FAB-MS (M+H)+ =520.

1. customThe reaction mixture, which has been partially evaporated
2. additionis poured onto a mixture of ice, 137 ml of sat. NH4Cl solution, 11 ml of 10% citric acid solution and 56 ml of methylene chloride, and methanol
3. additionis added until the precipitated solid
4. dissolutiondissolves
5. extractionThe aqueous phase is extracted with 2 portions of methylene chloride/methanol, approximately 10:1
6. washthe organic phases are washed with saline
7. dry with materialdried with Na2SO4
8. customevaporated
9. customtRet (I)=24.0 min