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

HRID 1915986노트

반응식

HRID 1915986 반응식
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

참가 물질

8

반응물 4

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

생성물 1

HCID 263703824-Methyl-1,2-dithiolane-4-carboxamide수율 60%

시약·촉매·용매 3

HCID 962Water용매HCID 3776Isopropanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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%

후처리

  1. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-f4d03334d3fa43a1bfda756d39852eb9
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08617524B2

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