Phenothiazine → Bis(trimethylsilyl)methylacrylate

HRID 480533

反応式

HRID 480533 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 18764809Bis(trimethylsilyl)methylacrylate

試薬・触媒・溶媒 2

HCID 21218Trioctylmethylammonium chloride触媒HCID 8008Butyronitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0e546afac53e4a3297d14375b599b8ea
出典データセット
uspto-grants-2003_11
特許番号
US06653048B2

関連ノート

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