
Journal of Organic Chemistry p. 3916 - 3926 (1989)
Update date:2022-09-26
Topics:
Dellaria, Joseph F.
Santarsiero, Bernard D.
A new synthetic method for the enantioselective preparation of α-amino acid derivatives is presented.The key step involves the diastereoselective alkylation of the new chiral glycine enolate synthons 7 and 8 providing alkylation adducts with de of > 97.6percent in good yields (73-90percent).The reactivities of the enolates of 7 and 8 were extraordinarily sensitive to the metal counterion and solvent.Experimental conditions are described to maintain high diastereoselectivities in the alkylation step for electrophiles varying from highly reactive (α-haloacetate esters) to less reactive (n-butyl iodide).The alkylation diastereoselectivities were established to be under kinetic control by equilibration experiments on selected alkylation products.A model is presented which hinges on an A(1,3) interaction between the termini of the N4-acyl protecting group and the C5-phenyl group of 7 and 8 which in turn dictates the ?-facial selectivity of the enolate.The model successfully accounts for the observed results and is corroborated by the conformation of an alkylation adduct as revealed by a single-crystal X-ray determination.A simple one-pot, three-step deprotection procedure provides the desired α-amino acid as the ethyl ester hydrochloride salts (60-80percent overall yield) with no attending racemization as determined by conversion of the amino acid esters to the corresponding (+)- or (-)-Mosher amides.
View Morezhuzhou zhongle chemical co. ltd.
Contact:+86-0731 28228409
Address:Zhuzhou, Hunan, China
Beijing Cooperate Pharmaceutical Co.,Ltd
website:http://www.cooperate-pharm.com/
Contact:86-01060279497
Address:No.507,Building 4,Tianhua Street, Biomedicine industrial Base
Nanjing Capatue Chemical Co., Ltd
Contact:+86-25-86371192 +86-025-85720158
Address:No.20 Jiangjun Avenue, Jiangning Economic & Technical Development Zone
Antaeus Bio-technology Co., LTD(expird)
Contact:021-31252569
Address:shanghai pudong
Yangzhou Siyu Chemical Co.,Ltd.
Contact:+86-514-87325867 13358126196
Address:Room 620 Exposition Pavilion,No. 98 Huaihai Road,Guangling District,Yangzhou City, Jiangsu Province
Doi:10.1002/anie.201302274
(2013)Doi:10.1021/jp909286t
(2010)Doi:10.1002/ejoc.200901110
(2010)Doi:10.1016/j.tet.2009.11.057
(2010)Doi:10.1139/v82-055
(1982)Doi:10.1016/j.ejmech.2009.11.006
(2010)