Synthesis of Myo-Inositols
315
1H, H-1), 3.73 (t, J ¼ 9.7 Hz, 1H, H-6), 3.68 (t, J ¼ 9.4 Hz, 1H, H-5), 3.61 (dd,
J ¼ 9.9, 2.7,Hz 1H, H-3), 3.42 (t, J ¼ 9.1 Hz, 1H, H-4); 13C NMR (75 MHz,
CD3OD): d 167.9 (COPh), 140.5, 134.3, 132.0, 130.9, 129.6, 129.4, 129.3, 128.7
(Ar-H), 83.5, 77.1, 76.7, 76.3, 75.1, 72.0, 71.9 (inositol ring carbons, CH2Ph).
L-9: mp. 134.0–135.58C; [a]2D5 259.6 (c 0.78, MeOH); Rf, MS(FAB), 1H
NMR, 13C NMR were identical to those of D-9.
D- and L-2-O-Benzoyl-6-O-benzyl-1,3,4,5-tetra-O-methoxymethyl-myo-inositol
(D-10 and L-10)
A mixture of the compound D-9 (50.0 mg, 0.13 mmol), chloromethyl methyl
ether (432 mL, 5.4 mmol), DIPEA (751 mL, 5.4 mmol), and 1,2-dichloroethane
(2 mL) was heated at 508C for 12 h. The mixture was diluted with EtOAc and
successively washed with aq NaHCO3 and brine. The organic phase was
dried (MgSO4), concentrated, and chromatographed to give compound D-10
(65.2 mg, 88.7%) as a colorless oil. Similarly, compound L-10 was prepared
from compound L-9.
D-10: Rf 0.60 (n-hexane:EtOAc, 1:1); [a]2D5 212.5 (c 0.25, CH2Cl2);
1
MS(FAB) ¼ m/z 551 (M þ H)þ, 573 (M þ Na)þ; H NMR (300 MHz, CDCl3): d
8.06–7.26 (m, 10H, Ar-H), 5.85 (t, J ¼ 2.6 Hz, 1H, H-2) 4.95–4.63 (m, 10H,
CH2Ph, OCH2OCH3), 3.98 (t, J ¼ 9.7 Hz, 1H, H-4), 3.87 (t, J ¼ 9.6 Hz, 1H,
H-5), 3.77 (dd, J ¼ 10.0, 2.6 Hz, 1H, H-3), 3.69 (dd, J ¼ 10.0, 2.6 Hz, 1H,
H-1), 3.60 (t, J ¼ 9.3 Hz, 1H, H-6), 3.43, 3.40, 3.38, 3.31 (4s, 12H,
OCH2OCH3); 13C NMR (75 MHz, CDCl3): d 166.5 (COPh), 139.0, 133.9,
130.7, 130.6, 129.2, 129.0, 128.3 (Ar-H), 99.5, 99.2, 96.6, 96.4 (OCH2OCH3),
81.6, 80.2, 78.7, 76.4, 75.6, 75.4, 70.4 (inositol ring carbons, CH2Ph), 57.4,
57.1, 56.7, 56.6 (OCH2OCH3).
L-10: [a]2D5 þ12.4 (c 0.20, CH2Cl2); Rf, MS(FAB), H NMR, 13C NMR were
1
identical to those of D-10.
D- and L-1,3,4,5-Tetra-O-methoxymethyl-myo-Inositol (D-11 and L-11)
A mixture of the compound D-10 (58.0 mg, 0.11 mmol), Pd(OH)2 on
charcoal (20%, 58 mg), and EtOH (1.5 mL) was hydrogenated (45 psi) at rt over-
night. The catalyst was filtered off through Celite and washed with CH2Cl2,
and the filtrate was evaporated. To a solution of the residue in MeOH (1 mL)
was added NaOMe (25% solution in MeOH, 2.4 mL, 11.0 mmol). After being
stirred for 19 h at rt, the solution was concentrated and chromatographed to
afford compound D-11 (31.9 mg, 85.0%) as an oil. Similarly, compound L-11
was prepared from compound L-10.
D-11: Rf 0.15 (EtOAc), 0.31 (CH2Cl2:MeOH, 9:1); [a]2D5 þ29.0 (c 0.65,
1
CHCl3); MS(FAB) ¼ m/z 357 (M þ H)þ, 379 (M þ Na)þ; H NMR (300 MHz,
CDCl3): d 4.87–4.74 (m, 8H, OCH2OCH3), 4.21 (t, J ¼ 2.6 Hz, 1H, H-2), 3.94
(t, J ¼ 9.6 Hz, 1H, H-4), 3.89 (t, J ¼ 9.3 Hz, 1H, H-5), 3.52–3.40 (m, 14H,
OCH2OCH3, H-1, H-3), 3.24 (t, J ¼ 9.2 Hz, 1H, H-6); 13C NMR (75 MHz,