P,P-Diphenylphosphinic azide → HCID 58976723、化合物
反応式
ClCCOC1C=C(C=C(OC)C=1OC)C(O)=O.[C:18]([O:22][C:23](=[O:39])[NH:24][C:25]1[CH:30]=[C:29]([O:31][CH3:32])[C:28]([O:33][CH3:34])=[C:27]([O:35][CH2:36][CH2:37][Cl:38])[CH:26]=1)([CH3:21])([CH3:20])[CH3:19].C1C=CC(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)=CC=1>C(O)(C)(C)C>[C:18]([O:22][C:23](=[O:39])[NH:24][C:25]1[CH:30]=[C:29]([O:31][CH3:32])[C:28]([O:33][CH3:34])=[C:27]([O:35][CH2:36][CH2:37][Cl:38])[CH:26]=1)([CH3:19])([CH3:21])[CH3:20]参加物
4
実験手順
[3-(2-Chloro-ethoxy)-4,5-dimethoxy-phenyl]-carbamic acid tert-butyl ester 3-(2-Chloro-ethoxy)-4,5-dimethoxy-benzoic acid (500 mg, 1.9 mmol), DPPA, (550 mg, 2 mmol), and TEA, (2 mmol), were combined in 5 mL t-butanol and refluxed for 5 h. The t-butanol was removed under vacuum and the residue purified by silica gel chromatography (5% methanol/DCM, affording 90 mg [3-(2-Chloro-ethoxy)-4,5-dimethoxy-phenyl]-carbamic acid tert-butyl ester. NMR CDCl3: 6.7 (d, 2H), 6.4 (bs, 1H), 4.3 (t, 3H), 3.85 (s, 3H), 3.80 (s, 3H), 3.82 (m, 2H), 1.5 (s, 9H).