Tributylamine → Bis-(tributylammonium) pyrophosphate

HRID 656673

反応式

HRID 656673 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-a6211fe6b3d5487391c8068dcbfabec6
出典データセット
uspto-grants-2011_12
特許番号
US08071739B2

関連ノート

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