Phenothiazine → Bis(trimethylsilyl)methylacrylate

HRID 1278529

反応式

HRID 1278529 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-3901f3841ab847a79d34516e6d4156e3
出典データセット
uspto-grants-2002_09
特許番号
US06444408B1

関連ノート

読み込み中…