Studies directed toward stereoselective synthesis of 1,3-amino alcohols via intramolecular amidomercuration /

Bibliographic Details
Main Author: Marman, Thomas Henry
Other Authors: Baldwin, T. O. (degree committee member.), Klein, L. L. (degree committee member.), Newcomb, M. E. (degree committee member.)
Format: Thesis Book
Language:English
Published: 1985.
Subjects:
Online Access:Link to ProQuest copy
Link to OAKTrust copy
ProQuest, Abstract

MARC

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099 |a 1985  |a Dissertation  |a M351 
100 1 |a Marman, Thomas Henry. 
245 1 0 |a Studies directed toward stereoselective synthesis of 1,3-amino alcohols via intramolecular amidomercuration / 
264 1 |c 1985. 
300 |a x, 123 leaves :  |b illustrations ;  |c 29 cm 
336 |a text  |b txt  |2 rdacontent 
337 |a unmediated  |b n  |2 rdamedia 
338 |a volume  |b nc  |2 rdacarrier 
500 |a "Major subject: Chemistry." 
500 |a Typescript (photocopy). 
500 |a Vita. 
502 |b Ph. D.  |c Texas A & M University  |d 1985 
504 |a Includes bibliographical references (leaves 118-122). 
520 3 |a The cyclization of the benzyl carbamate of 6-hepten-2-amine (31) with mercuric trifluoroacetate in nitromethane over a period of 20 h afforded, after borohydride reduction of the organomercurial, the benzyl carbamate of 2,6-dimethylpiperidine (30a) predominantly (98:2) as the cis diastereomer. Cyclization of 31 with mercuric acetate under similar conditions led to non-stereoselective (60:40 trans:cis) formation of 30a. The kinetically controlled product ratio of 95:5 trans:cis, obtained by cyclization of the benzyl carbamate of 5- hexen-2-amine (37) with mercuric trifluoroacetate for 15 min, was equilibrated, after 9 days of stirring, to a 40:60 trans:cis diastereomeric ratio of the 2,5-dimethylpyrrolidine carbamate. Cyclization precursor 31 was synthesized from 4-bromo-1-butene and ethyl acetoacetate in 5 steps with a 65% overall yield. The benzyl carbamate of 4,6-dimethyltetrahydro-1,3-oxazine (28) was formed by treatment of N-(benzyloxycarbonyl)aminomethyl 4-penten2-yl ether (27) with mercuric trifluoroacetate in a 40% yield or in a 60% yield with anhydrous mercuric nitrate in ethyl acetate after 15 min. A 73:27 cis:trans diastereomeric mixture was obtained. The organomercurial intermediate was equilibrated to a 6:94 cis:trans mixture after 46 h with mercuric nitrate in acetone. Cyclization precursor (27) was formed in two steps from benzyl carbamate in a 51% overall yield. The organomercurial formed from 31 was reduced in the presence of acrylonitrile with sodium borohydride to afford the alkylation product 89 in a 46% yield. Sodium borohydride reduction of the organomercurial from 27 with acrylonitrile led to a 32% yield of alkylation product 91. Reductive alkylation of the mercurial from 27 with - chloroacrylonitrile afforded the corresponding alkylation product (93) in a 16% yield. 
650 0 |a Amino alcohols. 
650 0 |a Stereochemistry. 
650 4 |a Major chemistry. 
655 7 |a Academic theses  |2 lcgft 
700 1 |a Baldwin, T. O.,  |e degree committee member. 
700 1 |a Harding, Kenn E.,  |e degree supervisor. 
700 1 |a Klein, L. L.,  |e degree committee member. 
700 1 |a Newcomb, M. E.,  |e degree committee member. 
710 2 |a Texas A & M University,  |e degree granting institution. 
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