Tributylamine → Tributyl ammonium pyrophosphate

HRID 1045343

反応式

HRID 1045343 の反応式
O.O.O.O.O.O.O.O.O.O.[O-:11][P:12]([O:15][P:16]([O-:19])([O-:18])=[O:17])(=[O:14])[O-:13].[Na+].[Na+].[Na+].[Na+].[CH2:24]([N:28]([CH2:33][CH2:34][CH2:35][CH3:36])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:25][CH2:26][CH3:27]>O.[NH+]1C=CC=CC=1.CO>[O-:13][P:12]([O:15][P:16]([O-:19])([O-:18])=[O:17])(=[O:11])[O-:14].[CH2:33]([NH+:28]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:34][CH2:35][CH3:36].[CH2:33]([NH+:28]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:34][CH2:35][CH3:36].[CH2:33]([NH+:28]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:34][CH2:35][CH3:36].[CH2:33]([NH+:28]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:34][CH2:35][CH3:36]

参加物

6

反応物 2

HCID 7622TributylamineHCID 3084150Sodium pyrophosphate decahydrate

生成物 1

HCID 21910867Tributyl ammonium pyrophosphate

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 4989215Pyridinium溶媒

実験手順

Tetrasodium diphosphate decahydrate (2.23 g, 5 mmol) was dissolved in water (50 mL), the solution was applied to a column of Dowex 50WX8 (100 mL) in the pyridinium form, and the column was washed with 300 mL water-methanol (1:1). The eluate was directly dropped into a cooled (ice water) and stirred solution of tri-n-butylamine (2.38 mL, 10 mmol) in methanol. The solution was evaporated to dryness and re-evaporated twice with methanol and finally with anhydrous DMF (30 mL) on an oil pump.

後処理

  1. washthe column was washed with 300 mL water-methanol (1:1)
  2. additionThe eluate was directly dropped into
  3. temperaturea cooled (ice water)
  4. customThe solution was evaporated to dryness
  5. customre-evaporated twice with methanol and finally with anhydrous DMF (30 mL) on an oil pump

出典と根拠

ORDレコード
ord-ee791794b29348c582575ae51307a739
出典データセット
uspto-grants-2013_10
特許番号
US08569259B2

関連ノート

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