Tributylphosphine → HCID 66960684、化合物

HRID 68987ノート

反応式

HRID 68987 の反応式
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]

参加物

7

反応物 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

生成物 1

HCID 66960684HCID 66960684、化合物収率 26.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-28b9692ca7a34b9c8b991784b78aa794
出典データセット
uspto-grants-2014_09
特許番号
US08822453B2

反応ノート

読み込み中…