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Pivalic acid → HCID 178447531、化合物

HRID 503701
ノート
印刷プレビュー

反応式

HRID 503701 の反応式
[Cl-].[Cl-].[CH3:3][C:4]1[C:8]([Zr+2:10][C:11]2([CH3:20])[C:15]([CH3:16])=[C:14]([CH3:17])[C:13]([CH3:18])=[C:12]2[CH3:19])([CH3:9])[C:7]([CH3:21])=[C:6]([CH3:22])[C:5]=1[CH3:23].[C:24]([OH:30])(=[O:29])[C:25]([CH3:28])([CH3:27])[CH3:26].C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:24]([O-:30])(=[O:29])[C:25]([CH3:28])([CH3:27])[CH3:26].[C:24]([O-:30])(=[O:29])[C:25]([CH3:28])([CH3:27])[CH3:26].[CH3:16][C:15]1[C:11]([Zr+2:10][C:8]2([CH3:9])[C:7]([CH3:21])=[C:6]([CH3:22])[C:5]([CH3:23])=[C:4]2[CH3:3])([CH3:20])[C:12]([CH3:19])=[C:13]([CH3:18])[C:14]=1[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6417Pivalic acidHCID 8471TriethylamineHCID 178426003HCID 178426003、化合物

生成物 1

HCID 178447531HCID 178447531、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of bis(pentamethylcyclopentadienyl)zirconium dichloride (0.865 g, 2.001 mmol) and pivalic acid (0.685 g, 6.710 mmol) in toluene (30 ml) at 40° C. was added triethylamine (0.726 g, 7.174 mmol) with stirring. A white precipitate formed immediately which was removed by filtration. The title compound was isolated as an off-white powder in 90% by evaporating the solvent and excess pivalic acid under vacuum at 65° C. The title compound such prepared exhibited purity above 98% based on NMR results. 1H NMR (toluene d8) δ1.83 (s, 30H), 1.30 (s, 18H).

後処理

  1. customA white precipitate formed immediately which
  2. customwas removed by filtration

出典と根拠

ORDレコード
ord-599b961384534c0ea3789c3808b75b6a
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776977B2

反応ノート

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