Reaktion #1737

ord-34b88de89a834c5b93af8ffabf69f38c

Reaktionsgleichung

CCCCCOc1cc2c(cc1C(=O)O)C(C)(C)CCC2(C)C
3-pentoxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalene-2-carboxylic acid
CCCCCOc1cc2c(cc1Br)C(C)(C)CCC2(C)C
6-bromo-7-pentoxy-1,1,4,4-tetramethyl-1,2,3,4-tetrahydro-naphthalene
[Li][C](C)(C)C
tert.butyl-lithium
O=C(OCc1ccccc1)c1ccc(O)nc1
benzyl 6-hydroxy-nicotinate
O=C=O
carbon dioxide
CCCCCOc1cc2c(cc1C(=O)Oc1ccc(C(=O)OCc3ccccc3)cn1)C(C)(C)CCC2(C)C
benzyl 6-(3-pentoxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-carbonyloxy)-nicotinate

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Vorschrift

In analogy to Example 1, by metallating 6-bromo-7-pentoxy-1,1,4,4-tetramethyl-1,2,3,4-tetrahydro-naphthalene with tert.butyl-lithium and reacting with carbon dioxide gas there was prepared 3-pentoxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalene-2-carboxylic acid (m.p. 67°-68° C., from hexane). Reaction of this acid with benzyl 6-hydroxy-nicotinate gave benzyl 6-(3-pentoxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-carbonyloxy)-nicotinate as a colorless oil. Subsequent hydrogenation yielded the desired end product 6-(3-pentoxy-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl-carbonyloxy)-nicotinic acid in white crystals, m.p. 132°-133° C. (from diethyl ether/hexane).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05726191uspto-grants-1998_03