Triphenylphosphine → HCID 178508341、化合物

HRID 646731ノート

反応式

HRID 646731 の反応式
[C:1]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH2:20][C:21]1[N:22]=[CH:23][C:24]([C:38]2[CH:39]=[C:40]([CH2:44]O)[CH:41]=[CH:42][CH:43]=2)=[N:25][C:26]=1[C:27]1[NH:31][C:30]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[N:29][N:28]=1.[C@@H:46]1([NH:55][S:56]([C:59]2[CH:64]=[CH:63][C:62]([N+:65]([O-:67])=[O:66])=[CH:61][C:60]=2[N+:68]([O-:70])=[O:69])(=[O:58])=[O:57])[C:54]2[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=2)[CH2:48][CH2:47]1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1.C(OCC)(=O)C>[NH2:20][C:21]1[N:22]=[CH:23][C:24]([C:38]2[CH:39]=[C:40]([CH:41]=[CH:42][CH:43]=2)[CH2:44][N:55]([C@@H:46]2[C:54]3[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=3)[CH2:48][CH2:47]2)[S:56]([C:59]2[CH:64]=[CH:63][C:62]([N+:65]([O-:67])=[O:66])=[CH:61][C:60]=2[N+:68]([O-:70])=[O:69])(=[O:58])=[O:57])=[N:25][C:26]=1[C:27]1[NH:31][C:30]([CH2:32][C:33]2[CH:1]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[N:29][N:28]=1

参加物

7

反応物 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 86607845N-[(1S)-2,3-dihydro-1H-inden-1-yl]-2,4-dinitrobenzen sulfonamideHCID 178508343HCID 178508343、化合物

生成物 1

HCID 178508341HCID 178508341、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Triphenylphosphine (47 mg, 0.17 mmol) was added to a stirred solution of {3-[5-amino-6-(5-phenyl-4H-1,2,4-triazol-3-yl) pyrazine-2-yl]phenyl}methanol (50 mg, 0.14 mmol) and N-[(1S)-2,3-dihydro-1H-inden-1-yl]-2,4-dinitrobenzen sulfonamide (60 mg, 0.16 mmol) in THF. Diethyl azodicarboxylate (31 mg, 0.17 mmol) was then added and mixture was stirred at ambient temperature 4 h. Ethyl acetate (20 mL) was added, and the organic layer was washed with saturated aqueous sodium chloride, and then dried (Na2SO4). Filtration and concentration followed by chromatography on silica gel afforded the title compound: MS (EI) for C35H29N9O6S: 704 (MH+).

後処理

  1. washthe organic layer was washed with saturated aqueous sodium chloride
  2. dry with materialdried (Na2SO4)
  3. filtrationFiltration and concentration

出典と根拠

ORDレコード
ord-0dfe80fcffe04a9cacdd4cee45d0e875
出典データセット
uspto-grants-2010_04
特許番号
US07704995B2

反応ノート

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