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Methanol → 1-(1-methyl-5-oxo-2(S)-pyrrolidinyl)-1,3-butanedione-3-oxime

HRID 21744
ノート
印刷プレビュー

反応式

HRID 21744 の反応式
[NH:1]1[C:5](=[O:6])[CH2:4][CH2:3][C@H:2]1[C:7]([OH:9])=O.CO.[CH3:12][C:13](=[N:15][OH:16])[CH3:14].[CH2:17]1COCC1>CCCCCC>[CH3:17][N:1]1[C:5](=[O:6])[CH2:4][CH2:3][C@H:2]1[C:7](=[O:9])[CH2:12][C:13](=[N:15][OH:16])[CH3:14]
参加物実験手順出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 7405L-Pyroglutamic AcidHCID 8028TetrahydrofuranHCID 67180Acetone, oxime

生成物 1

HCID 867487361-(1-methyl-5-oxo-2(S)-pyrrolidinyl)-1,3-butanedione-3-oxime

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

reacting the starting material, (S)-pyroglutamic acid, of formula (5), ##STR17## with methanol as the esterifying reagent at from -10° C. to 60° C. for from 4-to-48 hours, to prepare the (S)-pyroglutamic add ester of formula (6), ##STR18## wherein R1 is methyl; (b) reacting the compound of formula (6) with an excess of a salt of the dianion of acetone oxime in a solution of THF:hexane, at a temperature of from -10° C. to ambient temperature, with vigorous mixing of the reagents, to form the intermediate product, 1-(1-methyl-5-oxo-2(S)-pyrrolidinyl)-1,3-butanedione-3-oxime, which is not isolated, but which is cyclized and dehydrated by reaction with a strong acid at ambient-to-reflux temperature for from 0.5-to-3 hours, to produce the novel 5(S)-(3-methyl-5-isoxazolyl)-2-pyrrolidinone compound of formula (7), ##STR19## (c) reducing the compound of formula (7) with a reducing agent known to reduce lactams to cyclic amines, particularly an agent selected from the group consisting of lithium aluminum hydride, NaBH4 /BF3, NaBH4 /CH3SO3H, NaBH4 /camphor sulfonic acid, borane/dimethyl sulfide, and borane/THF, to give the 3-methyl-5-(2(S)-pyrrolidinyl)isoxazole compound of formula (8), ##STR20## which is not isolated; then (d) immediately treating the reaction product from step (c) with the N-alkylating agent formaldehyde and formic acid at ambient or an elevated temperature, and isolating the desired product of formula (1), wherein Alk is methyl, in high chiral purity.

出典と根拠

ORDレコード
ord-93d16b6a92ec419983390e3ee399b407
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05424444

反応ノート

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