Ammonia → 4-Methyl-1,2-dithiolane-4-carboxamide

HRID 1915986ノート

反応式

HRID 1915986 の反応式
ClC(OCC(C)C)=O.[CH3:9][C:10]1([C:15]([OH:17])=O)[CH2:14][S:13][S:12][CH2:11]1.C([N:20](CC)CC)C.N>C1COCC1.O.C(O)(C)C>[CH3:9][C:10]1([C:15]([NH2:20])=[O:17])[CH2:14][S:13][S:12][CH2:11]1

参加物

8

反応物 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 62365Isobutyl chloroformateHCID 200693114-Methyl-1,2-dithiolane-4-carboxylic acid

生成物 1

HCID 263703824-Methyl-1,2-dithiolane-4-carboxamide収率 60%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3776Isopropanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Alternatively, method (Ex. 5-b), 1.2 equivalents of isobutyl chloroformate are added, at 0° C., to a solution of 1 g of Compound 1 in THF with 1.2 equivalents of triethylamine. After 2 hours at room temperature, the reaction medium is added to a cooled solution of ammonia, either at 28% in water or at 2N in isopropanol. The medium is stirred at room temperature for the time required, and then concentrated under vacuum. The crude product is then taken up in toluene, to give Compound 2 after precipitation. Yield=60%

後処理

  1. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-f4d03334d3fa43a1bfda756d39852eb9
出典データセット
uspto-grants-2013_12
特許番号
US08617524B2

反応ノート

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