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BENZYL (4-BROMOBUTYL)CARBAMATE synthesis

5synthesis methods
-

Yield:101625-10-9 99.5%

Reaction Conditions:

with triphenylphosphine in dichloromethane;

Steps:

22.b 6-Amino-2-((2-methyl-1-(3-phenylpropanoylamino)propyl)hydroxyphosphinoyl)methylhexanoic acid

(b) The 4-benzyloxycarbonylamino-1-butanol (8.15 g) obtained in the above step (a) and carbon tetrabromide (15.12 g) were dissolved in methylene chloride (130.4 ml) and cooled with water. The mixture was added with triphenylphosphine (14.4 g) and returned to room temperature, and then stirred for 4 hours. The reaction system was concentrated under reduced pressure without any treatment, and the residue was purified by silica gel column chromatography (400 g, hexane:ethyl acetate=5:2) to obtain 1-benzyloxycarbonylamino-4-bromobutane (10.4 g, 99.5%). 1H-NMR(CDCl3): δ1.58-1.72(2H,m), 1.84-1.94(2H,m), 3.18-3.28(2H,dd), 3.42(2H,dd), 4.80(1H,s), 5.10(2H,s), 7.29-7.39(5H,m). EIMS(m/z): 286(M+).

References:

US6576627,2003,B1