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Triphenylphosphine → HCID 59571732、化合物

HRID 2194307
ノート
印刷プレビュー

反応式

HRID 2194307 の反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:38]=[CH:37][C:18]([CH2:19][N:20]2[C:32]3[CH:31]=[CH:30][CH:29]=[C:28]([O:33]CC=C)[C:27]=3[C:26]3[C:21]2=[CH:22][CH:23]=[CH:24][CH:25]=3)=[CH:17][C:16]=1[O:39][CH3:40].O1CCCC1CCO.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(O)=O>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:38]=[CH:37][C:18]([CH2:19][N:20]2[C:32]3[CH:31]=[CH:30][CH:29]=[C:28]([OH:33])[C:27]=3[C:26]3[C:21]2=[CH:22][CH:23]=[CH:24][CH:25]=3)=[CH:17][C:16]=1[O:39][CH3:40]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11776TriphenylphosphineHCID 119895722-(Oxolan-2-yl)ethan-1-olHCID 59571733HCID 59571733、化合物

生成物 1

HCID 59571732HCID 59571732、化合物

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 284Formic Acid溶媒

実験手順

10 g of 9-{4-[(5-methyl-2-phenyloxazole-4-yl)methoxy]-3-methoxybenzyl}-4-(allyloxy)-9H-carbazole was suspended in mixed solution (70 mL) of tetrahydrofuran-ethanol=4:1, 986 mg of triphenylphosphine, 84 mg of palladium acetate, and 2.1 mL of formic acid were added, and refluxed for 5 hours. The reaction mixture was allowed to cool, and then concentrated in vacuo, and the residue was crystallized from 10 mL of ethanol. The crystalline precipitate was isolated by filtration, washed with ethanol, dried under reduced pressure, and 8.96 g of the subject compound was prepared as pale yellow crystal.

後処理

  1. additionwere added
  2. temperaturerefluxed for 5 hours
  3. temperatureto cool
  4. concentrationconcentrated in vacuo
  5. customthe residue was crystallized from 10 mL of ethanol
  6. customThe crystalline precipitate was isolated by filtration
  7. washwashed with ethanol
  8. dry with materialdried under reduced pressure, and 8.96 g of the subject compound
  9. customwas prepared as pale yellow crystal

出典と根拠

ORDレコード
ord-53c25cbe7ceb46ad977763f2db5cdcb5
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329913B2

反応ノート

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