Sulfate, hydrogen → Di-tert-butyl (chloromethyl) phosphate

HRID 1521880

반응식

HRID 1521880 반응식
[P:1]([OH:13])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(=O)(O)[O-].[Na+].S([O-])(O)(=O)=O.S(Cl)(O[CH2:28][Cl:29])(=O)=O>O.ClCCl>[P:1]([O:13][CH2:28][Cl:29])([O:3][C:4]([CH3:6])([CH3:7])[CH3:5])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:2]

참가 물질

7

반응물 4

HCID 61778Sulfate, hydrogenHCID 429756Phosphoric acid, bis(1,1-dimethylethyl) esterHCID 516892Sodium BicarbonateHCID 2733556Chloromethyl chlorosulfate

생성물 1

HCID 11701630Di-tert-butyl (chloromethyl) phosphate수율 52.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a well stirred suspension of di-tert-butyl hydrogen phosphate (4.7 g, 22.47 mmol) in water (186 ml) was added sodium bicarbonate (7.5 g, 89.52 mmol) followed by tetra-n-butylammomium hydrogen sulphate (760 mg, 2.238 mmol). The reaction mixture was stirred at room temperature for 15 min. To the reaction mixture was added dichloromethane (112 ml) at 0° C. and it was stirred for 10 min followed by the addition of chloromethyl chlorosulphate (4.4 g, 26.85 mmol) in dichloromethane (75 ml) at same temperature. The resultant mixture was vigorously stirred overnight at room temperature. The organic layer was separated, washed with brine and evaporated under reduced pressure to yield 3.04 g of product as pale yellow oil.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 15 min
  2. stirringit was stirred for 10 min
  3. customThe organic layer was separated
  4. washwashed with brine
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-55e0ea5f6cef4a9894c21dc202e0dd64
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073955B2

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