Pyridine → Tris-(tributylammonium) pyrophosphate

HRID 1886506

反応式

HRID 1886506 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].N1C=CC=CC=1>O.CN(C)C=O>[O-:13][P:12]([O:15][P:16]([OH: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]

参加物

6

反応物 3

HCID 1049PyridineHCID 7622TributylamineHCID 3084150Sodium pyrophosphate decahydrate

生成物 1

HCID 22621555Tris-(tributylammonium) pyrophosphate

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒2 回

実験手順

Tetrasodium pyrophosphate decahydrate (4.46 g, 10 mmol) was dissolved in the minimum amount of water (about 50 mL) and passed though a column of AG50W X8 resin (100-200 mesh, 4×10 cm bed; a strongly-acidic, cation exchange, polystyrene resin) poured in water. The column was eluted with water and the eluent was collected in an ice-cooled flask until pH of the eluent approached neutrality. Tri-n-butylamine (Aldrich Gold Label, 7.1 mL, 30 mmol) was added to the eluent and the two phases were stirred vigorously until all of the amine dissolved. The resulting solution was lyophilized. The residue was co-evaporated twice with dry pyridine and once with dry dimethylformamide. The residue was dissolved in dry dimethylforamide (10 mL) and the resulting 1.0M solution was stored (for as long as one month) at 0° under argon until used.

後処理

  1. washThe column was eluted with water
  2. customthe eluent was collected in an ice-
  3. temperaturecooled flask until pH of the eluent
  4. dissolutiondissolved
  5. custom(for as long as one month)
  6. customat 0°

出典と根拠

ORDレコード
ord-b94a372ab2524d22b8f2d7ff6dd66968
出典データセット
uspto-grants-1992_09
特許番号
US05151507

関連ノート

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