Water → Zirconium tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionate)

HRID 7268

反応式

HRID 7268 の反応式
[CH3:1][C:2]([CH3:13])([C:4](=[O:12])[CH2:5][C:6](=[O:11])[C:7]([CH3:10])([CH3:9])[CH3:8])[CH3:3].[Cl-].[Cl-].[Cl-].[Cl-].[Zr+4:18].O.[OH-].[Na+]>CO>[CH3:1][C:2]([CH3:13])([CH3:3])/[C:4](/[OH:12])=[CH:5]/[C:6]([C:7]([CH3:10])([CH3:9])[CH3:8])=[O:11].[CH3:1][C:2]([CH3:13])([CH3:3])/[C:4](/[OH:12])=[CH:5]/[C:6]([C:7]([CH3:10])([CH3:9])[CH3:8])=[O:11].[CH3:1][C:2]([CH3:13])([CH3:3])/[C:4](/[OH:12])=[CH:5]/[C:6]([C:7]([CH3:10])([CH3:9])[CH3:8])=[O:11].[CH3:1][C:2]([CH3:13])([CH3:3])/[C:4](/[OH:12])=[CH:5]/[C:6]([C:7]([CH3:10])([CH3:9])[CH3:8])=[O:11].[Zr:18]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 707002,2,6,6-Tetramethyl-3,5-heptanedioneHCID 9856075Zirconium chloride (ZrCl4), (T-4)-

生成物 1

HCID 6287074Zirconium tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionate)収率 98.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To 177 g of methanol, 43.7 g (0.216 mol) of 2,2,6,6-tetramethyl-3,5-heptanedione of 91% purity was dropwise added with stirring. To the resulting solution, a solution, which had been obtained by dissolving 12.7 g (0.054 mol) of ZrCl4 of 99% purity in 218 g of methanol and cooled to room temperature, was added over a period of about 5 minutes. The reaction was conducted for 1 hour with stirring, and 590 g of water was added over a period of 50 minutes. Then, stirring was performed for 1 hour. The resulting solution was adjusted to pH 6.6 with a 20% NaOH solution. The resulting crystals were collected by centrifugation and then dried. Thus, 43.9 g (yield: 98.2%) of tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionato)zirconium was obtained.

後処理

  1. customTo the resulting solution, a solution, which had been obtained
  2. additionwas added over a period of about 5 minutes
  3. stirringwith stirring
  4. stirringThen, stirring
  5. waitwas performed for 1 hour
  6. customThe resulting crystals were collected by centrifugation
  7. customdried

出典と根拠

ORDレコード
ord-d031c2a1d4404c0f8c49a7f6d73e8050
出典データセット
uspto-grants-2006_08
特許番号
US07084306B2

関連ノート

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