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Bis(trimethylsilyl)chloromethane → Bis(trimethylsilyl)methylmethacrylate

HRID 1278527
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HRID 1278527 반응식
[CH3:1][Si:2]([CH:5]([Si:7]([CH3:10])([CH3:9])[CH3:8])Cl)([CH3:4])[CH3:3].[C:11]([O-:16])(=[O:15])[C:12]([CH3:14])=[CH2:13].[Na+]>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C1C2NC3C(=CC=CC=3)SC=2C=CC=1.C(#N)C>[CH3:1][Si:2]([CH:5]([O:16][C:11](=[O:15])[C:12]([CH3:14])=[CH2:13])[Si:7]([CH3:10])([CH3:9])[CH3:8])([CH3:4])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 552583Bis(trimethylsilyl)chloromethaneHCID 3255932Sodium methacrylate

생성물 1

HCID 18764812Bis(trimethylsilyl)methylmethacrylate수율 60%

시약·촉매·용매 3

HCID 7108Phenothiazine촉매HCID 21218Trioctylmethylammonium chloride촉매
HCID 6342
Acetonitrile
용매

실험 절차

Bis(trimethylsilyl)chloromethane (Aldrich) (14.68 g, 0.075 mole), sodium methacrylate (8.96 g, 0.0825 mole), Adogen 464 (Aldrich) (1.70 g), and phenothiazine (0.05 grams) were placed in a round bottom flask equipped with a condenser, mechanical stirrer and a nitrogen inlet. The flask was charged with 200 ml acetonitrile and heated to reflux while stirring. After 4 days, the mixture was filtered to remove the solids and the solvent was removed in a rotary evaporator. Fractional distillation under reduced pressure gave 10.90 grams (60% yield) of a clear liquid at 46-48° C. at 0.5 mm pressure.

후처리

  1. customequipped with a condenser, mechanical stirrer and a nitrogen inlet
  2. temperatureheated
  3. temperatureto reflux
  4. filtrationthe mixture was filtered
  5. customto remove the solids
  6. customthe solvent was removed in a rotary evaporator
  7. distillationFractional distillation under reduced pressure

출처 및 근거

ORD 기록
ord-e2da1c82b1f34324a34bedf6ba85f15a
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06444408B1

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