Triphenylphosphine → HCID 59469503、化合物

HRID 1719095ノート

反応式

HRID 1719095 の反応式
[CH2:1]([C:3]1[N:4]([C:28]2[CH:33]=[CH:32][C:31]([OH:34])=[CH:30][CH:29]=2)[C:5](=[O:27])[C:6]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[C:20]([C:25]#[N:26])=[CH:21][CH:22]=[CH:23][CH:24]=3)=[CH:15][CH:14]=2)=[C:7]([CH2:9][CH2:10][CH3:11])[N:8]=1)[CH3:2].[O:35]1[C:39]2([CH2:44][CH2:43][CH:42](O)[CH2:41][CH2:40]2)[O:38][CH2:37][CH2:36]1.N(C(OC(C)C)=O)=NC(OC(C)C)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(OCC)(=O)C.O1CCCC1>[O:35]1[C:39]2([CH2:44][CH2:43][CH:42]([O:34][C:31]3[CH:32]=[CH:33][C:28]([N:4]4[C:5](=[O:27])[C:6]([CH2:12][C:13]5[CH:18]=[CH:17][C:16]([C:19]6[C:20]([C:25]#[N:26])=[CH:21][CH:22]=[CH:23][CH:24]=6)=[CH:15][CH:14]=5)=[C:7]([CH2:9][CH2:10][CH3:11])[N:8]=[C:3]4[CH2:1][CH3:2])=[CH:29][CH:30]=3)[CH2:41][CH2:40]2)[O:38][CH2:37][CH2:36]1

参加物

7

反応物 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 5673521,4-Dioxaspiro(4.5)decan-8-olHCID 574608414'-{[2-Ethyl-1-(4-hydroxyphenyl)-6-oxo-4-propyl-1,6-dihydropyrimidin-5-yl]methyl}biphenyl-2-carbonitrile

生成物 1

HCID 59469503HCID 59469503、化合物収率 98%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 4′-{[2-ethyl-1-(4-hydroxyphenyl)-6-oxo-4-propyl-1,6-dihydropyrimidin-5-yl]methyl}biphenyl-2-carbonitrile (4.0 g), 1,4-dioxaspiro[4.5]decan-8-ol (2.82 g), diisopropyl azodicarboxylate (1.9 M in toluene, 3.2 mL), triphenylphosphine (4.67 g) and tetrahydrofuran (20 ml) was stirred at room temperature for 2 hr. The reaction mixture was diluted with ethyl acetate, successively washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel to give the title compound as a pale yellow amorphous solid (5.13 g, 98%).

後処理

  1. washsuccessively washed with water and saturated brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-62ff5446eef44759a5c98d1da5ddf479
出典データセット
uspto-grants-2010_09
特許番号
US07803940B2

反応ノート

読み込み中…