I Hyakunincho, Shinjuku-ku, Tokyo 160, Japan Preparation of 1 -azabenz[de]anthrone (27) was carried out by making use of a German Patent reaction. An improved procedure gave (27) easily and rapidly. Compound (27) underwent self-condensation via a zinc-catalysed method or an alkali-fusion procedure. The zinc-catalysed condensation product was separated into four isomers; 3,12-diazatetrabenzo[a,cd,j,lm]perylene ( 7 ) , 3,15-diazabenzo[rst]phenanthro[l,l O,9-cdelpentaphene (4), 5,17-diazadibenzo[a,rst] naphtho[8,1,2-cde] pentaphene (3), and 5,1O-diazabenzo[rst]phenaleno[l,2,3-de]pentaphene (6). The major component was (3). The reduced product after alkali-fusion condensation of (27) was separated into four isomers; ( 7 ) , (3), (6), and 5,14-diazadinaphtho[l,2,3-cd: 1 ',2',3'-lm]perylene ( 2 ) . The major component was ( 2 ) .The structures of the isomers were assigned from their oxidation products, m.p., u.v.-visible, i.r., and mass spectra. According to our assignments, (6) and possibly 5,14-diazatetrabenzo-[a,cd,lm,o] perylene (1 0) are new structural isomers of fused nanocyclic compounds whose parent aromatic hydrocarbons have not been prepared, though (10) has not actually been isolated.

A gas chromatographic (GC) method was developed for the determination of sucrose monoesters of fatty acids (mono-SuE) and sucrose acetate isobutyrate (SAIB) in food additive premixes. Mono-SuE and SAIB fractions were prepared by column chromatography with either a C8 or a silica gel solid-phase extraction column. The mono-SuE fraction was acetylated and applied to a wide-bore GC column (0.53 mm × 15 m) by splitless injection for determination. The SAIB fraction was applied to the GC column without derivatization. Gas chromatography/mass spectrometry was used to confirm the identity of GC peaks. The detection limits for mono-SuE and SAIB were 0.005 and 0.01%, respectively. Mono-SuE (C12, C14, C16, C18, and C18:1) and SAIB were found in commercial food additive premixes and some foods.

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Electron impact mass spectra were measured for five isomers of pyridinobenzanthrones and three isomers of benzobenzanthrones. The fragmentation pattern and intensity of M", [M -HI', [ M -CO]'+, [M -CO -H(or 2H)I" and [ M -CO -HCN]" (i = 1, 2) ions indicated remarkable differences and very interesting features according to the isomers with or without nitrogen and condensation positions of a pyridino or benzo ring to the benzanthrone skeleton. Further, the competition of decompositions through [ M -HI', [M -CO]" or [M -HCN] + * ions was confirmed by the observation of metastable ions and the appearance energies of fragment ions. Interesting observations from these results were expulsion of an H atom in close proximity to the area around an O=C group, a weak bonding interaction between sp2 C-H and an O=C group, inducing specific hydrogen rearrangement, and characteristic charge localization on heteroatoms.