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Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) → HCID 178483340、化合物

HRID 1906118
ノート
印刷プレビュー

反応式

HRID 1906118 の反応式
[F:1][B-:2]([F:5])([F:4])[F:3].C[O+](C)C.[CH3:10][N:11]([CH2:13][C-:14]1[CH:18]=[CH:17][CH:16]=[CH:15]1)[CH3:12].[CH-:19]1[CH:23]=[CH:22][CH:21]=[CH:20]1.[Fe+2:24]>C(Cl)Cl>[F:1][B-:2]([F:5])([F:4])[F:3].[CH3:10][N+:11]([CH2:13][C-:14]1[CH:18]=[CH:17][CH:16]=[CH:15]1)([CH3:19])[CH3:12].[CH-:19]1[CH:23]=[CH:22][CH:21]=[CH:20]1.[Fe+2:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 15764045cyclopenta-1,3-diene;1-cyclopenta-2,4-dien-1-yl-N,N-dimethylmethanamine;iron(2+)

生成物 1

HCID 178483340HCID 178483340、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(Trimethylammoniomethyl)ferricinium bis(tetrafluoroborate) was prepared by the following procedure. A slurry of 7.47 g of trimethyloxonium tetrafluoroborate (50.6 mmol) in 125 mL of CH2Cl2 was added to 10 mL of dimethylaminomethylferrocene in 100 mL of the same solvent. The resulting mixture was stirred for 16 hours and the solvent was removed under reduced pressure. The resulting residue was recrystallized from hot water to give 13.62 g of (trimethylammoniomethyl)ferrocene tetrafluoroborate as golden-yellow platelets. 1.32 g of the (trimethylammoniomethyl)ferrocene tetrafluoroborate (8 mmol) were added to a mixture of 0.864 g of p-benzoquinone (8 mmol) and 2.16 mL of 48% aqueous tetrafluoroboric acid (16 mmol) in 60 mL of diethyl ether. The resulting mixture was stirred for 15 minutes and filtered to give a dark blue-black residue which was washed with ether until the washings were colorless to remove quinhydrone and dried under reduced pressure to give 1.69 g of (trimethyl-ammoniomethyl)ferricinium bis(tetrafluoroborate) (3.9 mmol) as a navy-blue solid, which decomposed at high temperature without a characteristic melting point.

後処理

  1. customthe solvent was removed under reduced pressure
  2. customThe resulting residue was recrystallized from hot water

出典と根拠

ORDレコード
ord-75a8e90fb05f401a87fc18ed9391de01
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04650609

反応ノート

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