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Triphosgene → 1-(8-Bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepin-2-yl)-5,5-dimethylimidazolidin-2-one

HRID 1190625
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HRID 1190625 반응식
Br.[Br:2][C:3]1[CH:4]=[CH:5][C:6]2[C:12]3[N:13]=[C:14]([NH:16][C:17]([CH3:21])([CH3:20])[CH2:18][NH2:19])[S:15][C:11]=3[CH2:10][CH2:9][O:8][C:7]=2[CH:22]=1.Cl[C:24](Cl)([O:26]C(=O)OC(Cl)(Cl)Cl)Cl>O1CCCC1>[Br:2][C:3]1[CH:4]=[CH:5][C:6]2[C:12]3[N:13]=[C:14]([N:16]4[C:17]([CH3:20])([CH3:21])[CH2:18][NH:19][C:24]4=[O:26])[S:15][C:11]=3[CH2:10][CH2:9][O:8][C:7]=2[CH:22]=1
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참가 물질

4

반응물 2

HCID 94429TriphosgeneHCID 86652327N2-(8-bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepin-2-yl)-2-methylpropane-1,2-diamine hydrobromide

생성물 1

HCID 582042741-(8-Bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepin-2-yl)-5,5-dimethylimidazolidin-2-one수율 51%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Following the Example 356, N2-(8-bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepin-2-yl)-2-methylpropane-1,2-diamine hydrobromide was reacted with triphosgene in tetrahydrofuran and purified on silicagel column eluting with 50% of ethyl acetate in heptane to give 1-(8-bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepin-2-yl)-5,5-dimethylimidazolidin-2-one. Yield 51%. MS (ESI+): 393.9

후처리

  1. custompurified on silicagel column
  2. washeluting with 50% of ethyl acetate in heptane

출처 및 근거

ORD 기록
ord-fb51cb04ccc547c0b840b50c1c9b17c1
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673952B2

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