ORDER
REPRINTS
654
VASANTHAKUMAR AND SURESH BABU
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9.78; IR (gmax): 2108 cmꢁ1 (-COCHN2); H NMR (CDCl3, d): 3.1 (2H, d),
4.2 (2H, m), 4.5 (2H, d), 5.2 (1H, s), 5.4 (1H, br) and 7.2–7.7 (13H, m).
Na-Fmoc-valyldiazomethane (IIb): Yield, 85%; m.p., 124–125ꢀC; RfA,
0.69; RfB, 0.81; [a]D25 ꢁ 23.40 (c ¼ 1, CHCl3); Anal. Calc. for C21H21N3O3: C,
69.4; H, 5.81; N, 11.56; Found: C, 69.28; H, 5.92; N, 11.46; IR (gmax):
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2105 cmꢁ1 (-COCHN2); H NMR (CDCl3, d): 0.90 (6H, d), 1.75 (1H, m),
4.10 (1H, m), 4.25 (1H, m), 4.45 (2H, m), 5.30 (1H, s), 5.4 (1H, d) and
7.3–7.9 (8H, m).
Na-Fmoc-phenylglycinyldiazomethane (IIc): Yield, 90%; m.p., 148–
149ꢀC; RfA, 0.66; RfB, 0.80; [a]D25 ꢁ 32.3 (c ¼ 1, CHCl3); Anal. Calc. for
C24H29N3O3: C, 72.50; H, 4.81; N, 10.57; Found: C, 72.68; H, 4.87; N,
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10.6; IR (gmax): 2107 cmꢁ1 (-COCHN2); H NMR (CDCl3, d): 4.25 (2H,
m), 4.4 (2H, d), 5.1 (1H, s), 6.05 (1H, br) and 7.2–7.8 (13H, m).
Na-Fmoc-D-phenylglycinyldiazomethane (IId): Yield, 92%; m.p.,
153ꢀC; RfA, 0.7; RfB, 0.83; [a]D25 þ 32.3 (c ¼ 1, CHCl3); Anal. Calc. for
C24H29N3O3: C, 72.50; H, 4.81; N, 10.57; Found: C, 72.43; H, 4.90;
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N, 10.52; IR (gmax): 2106 cmꢁ1 (-COCHN2); H NMR (CDCl3, d): 4.2 (2H,
m), 4.5 (2H, d), 5.1 (1H, s), 6.05 (1H, br) and 7.2–7.8 (13H, m).
Na-Boc-alanyldiazomethane (IIe): Yield, 93%; m.p., 82ꢀC; RfA, 0.72;
RfB, 0.82; [a]2D5 ꢁ 21.7 (c ¼ 1, CHCl3); Anal. Calc. for C, 50.69; H, 7.08;
N, 19.70; Found: C, 50.80; H, 7.20; N, 19.47; IR (gmax): 2106 cmꢁ1
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(-COCHN2); H NMR (CDCl3, d): 1.05 (3H, d), 1.32 (9H, s), 4.21 (1H,
m), 5.25 (1H, s) and 5.5 (1H, br).
Na-Boc-valyldiazomethane (IIf ): Yield, 90%; m.p., 64ꢀC; RfA, 0.72;
RfB, 0.83; [a]D25 ꢁ 30.4 (c ¼ 1, CHCl3); Anal. Calc. for C11H19N3O3: C,
54.75; H, 7.93; N, 17.41; Found: C, 54.62; H, 7.78; N, 17.42; IR (gmax):
2107 cmꢁ1 (-COCHN2); 1H NMR (CDCl3, d): 0.92 (6H, d), 1.32 (9H, s), 1.75
(1H, m), 4.21 (1H, br), 5.20 (1H, s) and 5.42 (1H, br).
Na-Z-phenylalanyldiazomethane (IIg): Yield, 92%; m.p., 82–83ꢀC;
RfA, 0.68; RfB, 0.78; [a]D25 þ 48.2 (c ¼ 1, CHCl3); Anal. Calc. for
C18H17N3O3: C, 66.86; H, 5.29; N, 12.99; Found: C, 66.72; H, 5.35;
N, 12.86; IR (gmax): 2107 cmꢁ1 (-COCHN2); 1H NMR (CDCl3, d): 2.9
(2H, d), 4.45 (1H, m), 5.0 (2H, s), 5.22 (1H, s), 5.46 (1H, br) and 7.2–7.3
(10H, m).
Na-Z-alanyldiazomethane (IIh): Yield, 88%; m.p., 93–94ꢀC; RfA, 0.70;
RfB, 0.81; [a]2D5 ꢁ 50.3 (c ¼ 1, CHCl3); Anal. Calc. for C12H13N3O3: C, 58.29;
H, 5.29; N, 16.99; Found: C, 57.95; H, 5.13; N, 16.78; IR (gmax): 2107 cmꢁ1
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(-COCHN2); H NMR (CDCl3, d): 1.2 (3H, d), 4.26 (1H, m), 5.1 (2H, s),
5.25 (1H, s), 5.5 (1H, br) and 7.32 (5H, s).
Na-Z-phenylglycyldiazomethane (IIi): Yield, 86%; m.p., 83–84ꢀC; RfA,
0.69; RfB, 0.79; [a]D25 ꢁ 36.4 (c ¼ 1, CHCl3); Anal. Calc. for C17H15N3O3:
C, 66.01; H, 4.88; N, 13.58; Found: C, 65.72; H, 4.76; N, 13.72; IR