반응 #81338

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trifluoroacetic acid

N-(1,1-dimethylethoxycarbonyl)valine [11β,21-dihydroxy-3,20-dioxo-6α-methyl-17-propionyloxy-pregna-1,4-dien-21-yl] ester

→

valine [11β,21-dihydroxy-3,20-dioxo-6α-methyl-17-propionyloxy -pregna-1,4-dien-21-yl] ester trifluoroacetate

수율 80.0%

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후처리

1. 1
   온도Under initial cooling
2. 2
   기타Then, the trifluoroacetic acid is evaporated in a vacuum
3. 3
   workup.ADDITIONis added
4. 4
   기타evaporated to dryness in a vacuum
5. 5
   기타The residue is crystallized

실험 절차

Under initial cooling, 5 ml of trifluoroacetic acid is poured over 896 mg (1.42 mmol) of N-(1,1-dimethylethoxycarbonyl)valine [11β,21-dihydroxy-3,20-dioxo-6α-methyl-17-propionyloxy-pregna-1,4-dien-21-yl] ester, and it is stirred for 1-2 hours at room temperature. Then, the trifluoroacetic acid is evaporated in a vacuum. The residue is taken up in a little dichloromethane, 5 ml of toluene is added and then evaporated to dryness in a vacuum. The residue is crystallized. 728 mg (80%) of valine [11β,21-dihydroxy-3,20-dioxo-6α-methyl-17-propionyloxy -pregna-1,4-dien-21-yl] ester trifluoroacetate is obtained. Melting point 148° C.

출처