The naturally occurring dihydrohomopterin derivative 6-acetyl-2-amin0-7,8-dihydro-SH-pyrimido- [4,5-b] [I ,4]diazepin-4(3H)-one (1 ) has been synthesised from 1 -amino-4,4-diethoxypentan-3-01 (1 0) and 2-amino-6-chloro-5-nitropyrimidin-4(3H) -one (3). A novel tricyclic intermediate, 2,2a -di hydroxy-2-methyl -6 -nitro-1,2,2a,3,4,5hexa hydro-1,5,8,8b-tetra -ara -acenaphthylen -7 -one was isolated.