Potassium Acetate → (Acetoxymethyl)dimethoxymethylsilane

HRID 2363904

반응식

HRID 2363904 반응식
[C:1]([O-:4])(=[O:3])[CH3:2].[K+].Cl[CH2:7][SiH2:8][CH:9]([O:12][CH3:13])[O:10][CH3:11]>[Br-].C([P+](CCCC)(CCCC)CCCC)CCC.C(OCCOCCOCCCC)CCC>[C:1]([O:4][CH2:7][SiH2:8][CH:9]([O:12][CH3:13])[O:10][CH3:11])(=[O:3])[CH3:2]

참가 물질

5

반응물 2

HCID 517044Potassium AcetateHCID 57375894Chloromethyldimethoxymethylsilane

생성물 1

HCID 123920826(Acetoxymethyl)dimethoxymethylsilane수율 91%

시약·촉매·용매 2

HCID 76564Tetrabutylphosphonium bromide촉매HCID 8210Diethylene glycol dibutyl ether용매

실험 절차

Example 2 was repeated using potassium acetate (405 g, 4.13 mol) and (chloromethyl)dimethoxymethylsilane (535 g, 3.46 mol) as starting materials, tetrabutylphosphonium bromide (35.0 g, 10.3 mmol) as catalyst and diethylene glycol dibutyl ether (525 mL) as solvent. After the reaction, the product was distilled at 10 mbar (head), 61-70° C. (head) and 80-119° C. (pot) through a packed column (20 cm) to obtain 560 g (3.14 mol, 91% of theory) of (acetoxymethyl)-dimethoxymethylsilane in the distillate; purity 98.0% (GC area %). The solvent then started to pass over at 10 mbar (head), 118° C. (head) and 124° C. (pot); by distilling over about 10 g of solvent, the (acetoxymethyl)dimethoxymethylsilane was fully removed from the residue. The solvent, potassium chloride, excess potassium acetate and the phase transfer catalyst (in the form of the bromide, chloride and acetate salt of tetrabutylphosphonium) remained in the residue.

후처리

  1. customAfter the reaction
  2. distillationthe product was distilled at 10 mbar (head), 61-70° C. (head) and 80-119° C. (pot) through a packed column (20 cm)

출처 및 근거

ORD 기록
ord-1ae6698a9fea467c960df6ac1a9893dd
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08692012B2

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