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Ammonium hexafluorophosphate → 3-Benzyl-1-methoxy-4,5-dimethylimidazolium hexafluorophosphate

HRID 1072768
ノート
印刷プレビュー

反応式

HRID 1072768 の反応式
[I-].[CH2:2]([N:9]1[C:13]([CH3:14])=[C:12]([CH3:15])[N+:11]([O:16][CH3:17])=[CH:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[F:18][P-:19]([F:24])([F:23])([F:22])([F:21])[F:20].[NH4+]>O>[F:18][P-:19]([F:24])([F:23])([F:22])([F:21])[F:20].[CH2:2]([N:9]1[C:13]([CH3:14])=[C:12]([CH3:15])[N+:11]([O:16][CH3:17])=[CH:10]1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
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 9793912Ammonium hexafluorophosphateHCID 178502610HCID 178502610、化合物

生成物 1

HCID 1785026093-Benzyl-1-methoxy-4,5-dimethylimidazolium hexafluorophosphate

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Crude iodide 2 was taken up in deionized (DI) water, which separated the product from small amounts of a dark, insoluble residue. The water solution was decanted to a second flask and a solution of ammonium hexafluorophosphate (950 mg, ca. 5.8 mmol) in 10 mL of DI water was added in portions. An oil separated during the addition, and the supernatant solution was decanted out. The oil was crushed in cold (0° C.), and subsequently recrystallized in methanol. Yield: 1.3 g (73% from 1). 1H-NMR (δ, CDCl3): 8.67 (s, 1H, N—CH—N); 7.39 (m, 3H, C6H5); 7.29 (d, 2H, C6H5); 5.24 (s, 2H, NCH2); 4.21 (s, 3H, OCH3); 2.27 (s, 3H, CH3); 2.17 (s, 3H, CH3).

後処理

  1. customseparated the product from small amounts of a dark, insoluble residue
  2. customThe water solution was decanted to a second flask
  3. customAn oil separated during the addition
  4. customthe supernatant solution was decanted out
  5. customThe oil was crushed in cold (0° C.)
  6. customsubsequently recrystallized in methanol

出典と根拠

ORDレコード
ord-6b368fc424bb42e48e1214a6f2742362
出典データセット
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06911546B2

反応ノート

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