Ethanol → Tetraethylammonium Hydroxide

HRID 348536

反応式

HRID 348536 の反応式
S(O[CH2:8][CH3:9])(OCC)(=O)=[O:2].[CH2:10]([N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])[CH3:11].C(O)C.[OH-].[Na+]>>[OH-:2].[CH2:10]([N+:12]([CH2:8][CH3:9])([CH2:15][CH3:16])[CH2:13][CH3:14])[CH3:11]

参加物

5

反応物 4

HCID 702EthanolHCID 6163Diethyl SulfateHCID 8471TriethylamineHCID 14798Sodium Hydroxide

生成物 1

HCID 6509Tetraethylammonium Hydroxide収率 410.2%

反応条件

温度
140 °C

実験手順

To a 1.5 L autoclave equipped with a stirrer and a heating means were added 154 g (1.0 mol) of diethyl sulfate, 101 g (1.0 mol) of triethyl amine and 690 g (15 mol) of ethanol. Stirring was initiated after the autoclave was sealed. The autoclave was heat to 140° C., and pressure was 1.0 MPa. The reaction was kept at 140° C. for 4 h. Then the reaction mixture was cooled to room temperature and discharged into a 1 L three-necked flask. 80 g (2.0 mol) of sodium hydroxide was added thereto. The reaction mixture was heated at 45° C. for 4 h while stirring. After filtration, part of ethanol was distilled off from the filtrate. Then 500 g of water was added while ethanol was distilled off (part of water was entrained out), to give 604 g of tetraethyl ammonium hydroxide solution. The content of tetraethyl ammonium hydroxide was found as 23.3 wt.-% and the total reaction yield was 95.7%.

後処理

  1. customTo a 1.5 L autoclave equipped with a stirrer
  2. customwas sealed
  3. temperatureThen the reaction mixture was cooled to room temperature
  4. customdischarged into a 1 L three-necked flask
  5. temperatureThe reaction mixture was heated at 45° C. for 4 h
  6. stirringwhile stirring
  7. filtrationAfter filtration, part of ethanol
  8. distillationwas distilled off from the filtrate
  9. additionThen 500 g of water was added while ethanol
  10. distillationwas distilled off (part of water was entrained out)

出典と根拠

ORDレコード
ord-f896af9aea1943f48e0b6ee1c9c6414a
出典データセット
uspto-grants-2007_02
特許番号
US07176333B2

関連ノート

読み込み中…