Tributylamine → Bis-(tributylammonium) pyrophosphate

HRID 656673

반응식

HRID 656673 반응식
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]

참가 물질

5

반응물 2

HCID 7622TributylamineHCID 3084150Sodium pyrophosphate decahydrate

생성물 1

HCID 86637539Bis-(tributylammonium) pyrophosphate

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-a6211fe6b3d5487391c8068dcbfabec6
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071739B2

연결된 노트

불러오는 중…