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2,6-Di-tert-butylphenol → HCID 66586998、化合物

HRID 870116
ノート
印刷プレビュー

反応式

HRID 870116 の反応式
BrC1C=C[C:12]2[C:11]3[C:6](=CC(Br)=[CH:9][CH:10]=3)[C:5]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][Br:29])([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][Br:22])[C:4]=2C=1.[C:30]([C:34]1[CH:39]=[CH:38][CH:37]=[C:36](C(C)(C)C)[C:35]=1O)([CH3:33])(C)C.[CH2:45](C([Sn])=C(CCCC)CCCC)[CH2:46]CC.[F-].[K+]>CCOCC.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1(C)C=CC=CC=1>[Br:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][C:5]1([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][Br:29])[C:35]2[CH:36]=[C:37]([CH:45]=[CH2:46])[CH:38]=[CH:39][C:34]=2[C:30]2[C:4]1=[CH:12][C:11]([CH:10]=[CH2:9])=[CH:6][CH:33]=2
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 4

HCID 314052,6-Di-tert-butylphenolHCID 522689Potassium FluorideHCID 218679302,7-Dibromo-9,9-bis(6-bromohexyl)-9H-fluoreneHCID 53438229Tri(butyl)vinyltin

生成物 1

HCID 66586998HCID 66586998、化合物

試薬・触媒・溶媒 3

HCID 178418476
HCID 178418476、化合物
触媒
HCID 1140Toluene溶媒
HCID 3283Diethyl Ether溶媒

反応条件

温度
100 °C

実験手順

A flask with a stirring bar was charged with a mixture of compound 1 (1.000 g, 1.54 mmol), PdCl2(PPh3)2 (0.0588 g, 0.065 mmol), a few crystals of 2,6-ditert-butylphenol, and toluene (15.0 mL). The mixture was heated to 100° C. under nitrogen, and tributylvinyltin (1.125 g, 3.534 mmol) was added dropwise. The mixture was further heated for 23 hours. It was subsequently diluted with 60 mL of ether and treated with KF solution (˜10%). The mixture was stirred for 20 hours and followed by filtration to remove the insoluble solid. The organic layer was washed with water and dried over anhydrous MgSO4. After removal of the solvent, the residue was purified by column chromatography with n-hexane as eluent to afford 0.650 g of compound 2.

後処理

  1. temperatureThe mixture was further heated for 23 hours
  2. filtrationfollowed by filtration
  3. customto remove the insoluble solid
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous MgSO4
  6. customAfter removal of the solvent
  7. customthe residue was purified by column chromatography with n-hexane as eluent

出典と根拠

ORDレコード
ord-4bbe3177a8784ef1a311010b986c19fd
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969509B2

反応ノート

読み込み中…

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