Tributylamine → Bis-(tributylammonium) pyrophosphate

HRID 500305

反応式

HRID 500305 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.CCO>[O-:13][P:12]([O:15][P:16]([OH:19])([OH: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]

参加物

5

反応物 2

HCID 7622TributylamineHCID 3084150Sodium pyrophosphate decahydrate

生成物 1

HCID 86637539Bis-(tributylammonium) pyrophosphate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Tetrasodium diphosphate decahydrate (1.5 g, 3.4 mmol) was dissolved in water (34 ml) and the solution was applied to a column of dowex in the H+ form. The column was eluted with water. The eluent dropped directly into a cooled (ice bath) and stirred solution of tri-n-butylamine (1.6 ml, 6.8 mmol) in EtOH (14 ml). The column was washed until the pH of the eluent increased to 6. The aq. ethanol solution was evaporated to dryness and then co-evaporated twice with ethanol and twice with anhydrous DMF. The residue was dissolved in DMF (6.7 ml). The pale yellow solution was stored over 4 Å molecular sieves.

後処理

  1. washThe column was eluted with water
  2. additionThe eluent dropped directly into
  3. temperaturea cooled (ice bath)
  4. washThe column was washed until the pH of the eluent
  5. temperatureincreased to 6
  6. customThe aq. ethanol solution was evaporated to dryness
  7. dissolutionThe residue was dissolved in DMF (6.7 ml)

出典と根拠

ORDレコード
ord-01b4592527884288922f7f45012871e2
出典データセット
uspto-grants-2010_08
特許番号
US07771973B2

関連ノート

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