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

HRID 882349

반응식

HRID 882349 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate수율 59.3%

시약·촉매·용매 3

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 962Water용매HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3119adfdbd844883a243af3c9a9828b8
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993614B2

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