Triphenylphosphine → HCID 59469503, 화합물

HRID 1674426노트

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HRID 1674426 반응식
[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

참가 물질

7

반응물 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

생성물 1

HCID 59469503HCID 59469503, 화합물수율 98%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-3ee142a258cf42978a3721bd6f28fdba
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998968B2

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