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Tri-o-tolylphosphine → HCID 22132398、化合物

HRID 1856685
ノート
印刷プレビュー

反応式

HRID 1856685 の反応式
C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.[CH2:23]1[CH2:32][O:31][C:30]2[CH:29]=[CH:28][C:27](Br)=[CH:26][C:25]=2[O:24]1.[N:34]1[CH:39]=[CH:38][CH:37]=[C:36]([CH2:40][CH2:41][CH:42]([OH:45])[CH:43]=[CH2:44])[CH:35]=1>C(N(CC)CC)C.C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[O:31]1[C:30]2[CH:29]=[CH:28][C:27]([CH2:44][CH2:43][C:42](=[O:45])[CH2:41][CH2:40][C:36]3[CH:35]=[N:34][CH:39]=[CH:38][CH:37]=3)=[CH:26][C:25]=2[O:24][CH2:23][CH2:32]1.[O:31]1[C:30]2[CH:29]=[CH:28][C:27](/[CH:44]=[CH:43]/[CH:42]([OH:45])[CH2:41][CH2:40][C:36]3[CH:35]=[N:34][CH:39]=[CH:38][CH:37]=3)=[CH:26][C:25]=2[O:24][CH2:23][CH2:32]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 80271Tri-o-tolylphosphineHCID 1041416-Bromo-1,4-benzodioxaneHCID 17866850HCID 17866850、化合物

生成物 2

HCID 22132398HCID 22132398、化合物HCID 22132429HCID 22132429、化合物

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒
HCID 6342
Acetonitrile
溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
80 °C

実験手順

A mixture of palladium(II) acetate (0.112 g), tri-o-tolylphosphine (0.304 g), 3,4-ethylenedioxybromobenzene (1.075 g) and (±)-5-(pyridin-3-yl)-1-penten-3-ol (0.815 g, Example 1a)) in triethylamine (10 ml) in acetonitrile (30 ml) was heated at 80° C. for 3 hours and 30 minutes. The mixture was cooled to room temperature and filtered through Celite® and the filtrate concentrated under reduced pressure. The residue was redissolved in ethyl acetate and the solution washed with water then dried over anhydrous magnesium sulfate. The solution was then filtered and concentrated under reduced pressure. The residue was purified by column chromatography over silica eluting with hexane:acetone (3:1) then (2:1) to give firstly 1-(benzo-1,4-dioxan-6-yl)-5-(pyridin-3-yl)-3-pentanone as an oil (0.812 g) and secondly (±)-trans-1-(benzo-1,4-dioxan-6-yl)-5-(pyridin-3-yl)-pent-1-en-3-ol as an oil (0.252 g).

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered through Celite®
  3. concentrationthe filtrate concentrated under reduced pressure
  4. dissolutionThe residue was redissolved in ethyl acetate
  5. washthe solution washed with water
  6. dry with materialthen dried over anhydrous magnesium sulfate
  7. filtrationThe solution was then filtered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by column chromatography over silica eluting with hexane:acetone (3:1)

出典と根拠

ORDレコード
ord-29f913015d1e467fabab1b28a67e44cd
出典データセット
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06143751

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート