Sodium Bicarbonate → Di-tert-butyl (chloromethyl) phosphate

HRID 882349

反応式

HRID 882349 の反応式
[C:1]([O:5][P:6]([O-:13])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])([CH3:4])([CH3:3])[CH3:2].[K+].C(=O)(O)[O-].[Na+].S(Cl)(O[CH2:24][Cl:25])(=O)=O>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O.C(Cl)Cl>[P:6]([O:13][CH2:24][Cl:25])([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7]

参加物

7

反応物 3

HCID 516892Sodium BicarbonateHCID 2733556Chloromethyl chlorosulfateHCID 23674467Potassium di-tert-butyl phosphate

生成物 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate収率 59.3%

試薬・触媒・溶媒 3

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of potassium di-tert-butylphosphate (2.45 g, 9.51 mmol), sodium bicarbonate (3.19 g, 38.0 mmol) and tetrabutylammonium hydrogen sulfate (340.2 mg, 0.972 mmol) in water (80 mL), was added methylene chloride (50 mL). The mixture was cooled to 0° C. and stirred vigorously under argon for 10 min. Chloromethyl chlorosulfate (1.92 g, 1.2 mL, 11.6 mmol) in methylene chloride (30 mL) was added slowly and the reaction was stirred at room temperature overnight. The organic layer was separated, washed with brine and dried over anhydrous sodium sulfate and concentrated to give di-tert-butyl chloromethyl phosphate as a colorless oil (1.46 g, 59% yield).

後処理

  1. stirringthe reaction was stirred at room temperature overnight
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-3119adfdbd844883a243af3c9a9828b8
出典データセット
uspto-grants-2015_03
特許番号
US08993614B2

関連ノート

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