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3
858
Mielniczak and Bopusinski
´
Cis-2-amino-2-oxo-4-methyl-1,3,2-dioxaphosphinane (8). (i) Following
the procedure (a) trans-phosphite 6 (90% trans-, 10% cis-) (1.36 g,
1
0 mmol), iodoform (3.93 g, 10 mmol) 1, and gaseous ammonia gave
.5 g of the product as a mixture of cis-8 (89%) ꢀ 6.3 and trans-8
1
3
11%) ꢀ 9.2 isomers identified by P NMR integrated spectrum. From
1
(
this a (0.93 g, 70%) of cis-8 P NMR (EtOD) ꢀ 6.4 m.p.: 127–128 C;
3
1
ꢁ
[23]
ꢁ
31
Lit. m.p.: 128–130 C, ꢀ P 6.0) was isolated by fractional crystalliza-
(
tion from ethanol-ethyl acetate. MS(FAB) m/z 152 [M þ 1]. (ii) Following
the procedure (b) trans-phosphite 6 (76% trans-, 24% cis-) (0.13 g,
1
cis-6 ꢀ 6.75 (75%) and trans-6 ꢀ 9.68 (25%) identified by P NMR.
mmol) of 1 and 12 mL of liquid ammonia gave a mixture of amidate
3
1
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