反应详情

To a cooled solution (−5° C.) of 5-(N-methyl-3-tert-butoxycarbonylaminopropyl)-benzene-1,3-dicarboxylic acid diethyl ester (100 mg) in tetrahydrofuran (2 mL) was slowly added a 1M solution of lithium aluminium hydride in diethyl ether (0.55 mL). 10 minutes after the end of the addition, sodium sulfate decahydrate was added until gas evolution ceased. The solid was filtered off, washed twice with ethyl acetate and the combined organic solutions were concentrated in vacuo to give 5-(N-methyl-3-tert-butoxycarbonylaminopropyl)-1,3-bis-(hydroxymethyl)-benzene (66.8 mg) as a viscous oil:

1. additionwas added until gas evolution
2. filtrationThe solid was filtered off
3. washwashed twice with ethyl acetate
4. concentrationthe combined organic solutions were concentrated in vacuo