Tributylphosphine → HCID 66960684, 화합물

HRID 68987노트

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HRID 68987 반응식
C(P(CCCC)CCCC)CCC.N(C(N1CCCCC1)=O)=NC(N1CCCCC1)=O.[N+:32]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[S:41]([NH:44][CH2:45][CH2:46][N:47]1[CH:56]=[CH:55][C:54]2[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=2)[C:48]1=[O:57])(=[O:43])=[O:42])([O-:34])=[O:33].[CH2:58]([N:60]1[C:66](=[O:67])[C:65]([CH3:69])([CH3:68])[C:64](=[O:70])[N:63]([CH3:71])[C:62]2[CH:72]=[C:73]([CH2:76][CH2:77][CH2:78]O)[CH:74]=[CH:75][C:61]1=2)[CH3:59]>O.C1(C)C=CC=CC=1>[CH2:58]([N:60]1[C:66](=[O:67])[C:65]([CH3:69])([CH3:68])[C:64](=[O:70])[N:63]([CH3:71])[C:62]2[CH:72]=[C:73]([CH2:76][CH2:77][CH2:78][N:44]([CH2:45][CH2:46][N:47]3[CH:56]=[CH:55][C:54]4[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=4)[C:48]3=[O:57])[S:41]([C:36]3[CH:37]=[CH:38][CH:39]=[CH:40][C:35]=3[N+:32]([O-:34])=[O:33])(=[O:42])=[O:43])[CH:74]=[CH:75][C:61]1=2)[CH3:59]

참가 물질

7

반응물 4

HCID 13831TributylphosphineHCID 730421,1'-(Azodicarbonyl)dipiperidineHCID 669613052-nitro-N-[2-(1-oxo-1H-isoquinolin-2-yl)-ethyl]-benzenesulfonamideHCID 706568861-Ethyl-7-(3-hydroxy-propyl)-3,3,5-trimethyl-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione

생성물 1

HCID 66960684HCID 66960684, 화합물수율 26.5%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

Tributyl phosphine (1.2 ml) and 1,1′-(azodicarbonyl)dipiperidine (1.17 g) were added to a toluene solution (100 ml) of 2-nitro-N-[2-(1-oxo-1H-isoquinolin-2-yl)-ethyl]-benzenesulfonamide (1.39 g), and 1-ethyl-7-(3-hydroxy-propyl)-3,3,5-trimethyl-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione (0.94 g). The mixture was stirred overnight. Water was added to the reaction mixture, followed by extraction using ethyl acetate. The organic layer was washed with water and saturated saline, dried with magnecium sulfate, and condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→1:0). The purified product was condensed under reduced pressure to produce the title compound (0.54 g) as a white amorphous.

후처리

  1. extractionfollowed by extraction
  2. washThe organic layer was washed with water and saturated saline
  3. dry with materialdried with magnecium sulfate, and condensed under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→1:0)
  5. customcondensed under reduced pressure

출처 및 근거

ORD 기록
ord-28b9692ca7a34b9c8b991784b78aa794
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822453B2

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