Phenothiazine → Bis(trimethylsilyl)methylacrylate

HRID 480533

반응식

HRID 480533 반응식
[CH3:1][Si:2]([CH:5]([Si:7]([CH3:10])([CH3:9])[CH3:8])Cl)([CH3:4])[CH3:3].[C:11]([O-:15])(=[O:14])[CH:12]=[CH2:13].[Na+].C1C2NC3C(=CC=CC=3)SC=2C=CC=1>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C(#N)CCC>[CH3:1][Si:2]([CH:5]([O:15][C:11](=[O:14])[CH:12]=[CH2:13])[Si:7]([CH3:10])([CH3:9])[CH3:8])([CH3:4])[CH3:3]

참가 물질

6

반응물 3

HCID 7108PhenothiazineHCID 552583Bis(trimethylsilyl)chloromethaneHCID 4068533Sodium acrylate

생성물 1

HCID 18764809Bis(trimethylsilyl)methylacrylate

시약·촉매·용매 2

HCID 21218Trioctylmethylammonium chloride촉매HCID 8008Butyronitrile용매

실험 절차

Bis(trimethylsilyl)chloromethane (Aldrich) 39 g, 0.2 mole), sodium acrylate (28 g, 0.3 mole), Adogen 464 (Aldrich) (6.96 g), and phenothiazine (0.10 grams) were placed in a round bottom flask equipped with a condenser, mechanical stirrer and a nitrogen inlet. The flask was charged with 100 ml of butyronitrile and heated to reflux while stirring. After 6 hours, the mixture was diluted with 150 ml hexanes and filtered to remove the solids. The solvents were removed under reduced pressure. Fractional distillation of the residue under reduced pressure gave 35.5 grams 975%) of the desired product at 45-58° C. at 0.5 mm pressure.

후처리

  1. customequipped with a condenser, mechanical stirrer and a nitrogen inlet
  2. temperatureheated
  3. temperatureto reflux
  4. filtrationfiltered
  5. customto remove the solids
  6. customThe solvents were removed under reduced pressure
  7. distillationFractional distillation of the residue under reduced pressure

출처 및 근거

ORD 기록
ord-0e546afac53e4a3297d14375b599b8ea
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06653048B2

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