Nitrogen → HCID 86747832、化合物

HRID 2399440ノート

反応式

HRID 2399440 の反応式
N#N.[OH:3][CH2:4][CH2:5][CH2:6][CH2:7][Si:8]([CH3:19])([CH3:18])[O:9][Si:10]([CH3:17])([CH3:16])[CH2:11][CH2:12][CH2:13][CH2:14][OH:15].N1C=CC=CC=1.Cl[C:27]([O:29]C=C)=[O:28]>C(Cl)Cl.C(#N)C>[C:27](=[O:28])([OH:29])[O:15][CH:14]=[CH2:13].[OH:15][CH2:14][CH2:13][CH2:12][CH2:11][Si:10]([CH3:17])([CH3:16])[O:9][Si:8]([CH3:18])([CH3:19])[CH2:7][CH2:6][CH2:5][CH2:4][OH:3]

参加物

7

反応物 4

HCID 947NitrogenHCID 1049PyridineHCID 78808Vinyl chloroformateHCID 27693461,3-Bis(4-hydroxybutyl)tetramethyldisiloxane

生成物 1

HCID 86747832HCID 86747832、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

A 500 ml 3-neck, round bottom flask equipped with a reflux condenser, a mechanical stirrer, a thermometer, a dropping funnel and a N2 blanket, is charged with 69.5 g (0.25 mole) of 1,3-bis(4-hydroxybutyl) tetramethyl disiloxane (Silar Lab.), pyridine, 19.5 g and 300 ml of methylene chloride. The contents are cooled down to between 0 and 5 degrees C. by an ice bath. Through the dropping funnel 25.3 g (0.25 mole) of vinyl chloroformate in 50ml of methylene chloride is added dropwise into the flask at a rate such that the temperature is maintained between 0 and 5 degrees C. The contents are then stirred for another 4 hours and then passed through a silica gel column. The eluents are condensed and injected in 6-8 gram portions into a reverse phase high performance liquid chromatography unit (Waters), using acetonitrile as solvent. Three fractions are collected. The major (center) fraction from each injection is collected and condensed to give 1,3-bis(4-hydroxybutyl)tetramethyl disiloxane monovinyl carbonate. The monovinyl carbonate product (34.8 g or 0.1 mole) is charged into a flask as already described, along with 8.0 g of pyridine, 50 mg of hydroquinone and 200 ml of chloroform. The contents are cooled down to between 0 and 5 degrees C. Through a dropping funnel, 10.5 g (0.1 mole) of methacryloyl chloride in 50 ml of chloroform is added into the flask at such a rate that the temperature is maintained between 0 and 5 degrees C. The contents are stirred continuously for 4 hours and then passed through a silica gel column. The contents are then condensed and distilled under reduced pressure to give the named product. Hydroquinone (50 mg) is added into the named product.

後処理

  1. customA 500 ml 3-neck, round bottom flask equipped with a reflux condenser, a mechanical stirrer
  2. temperatureThe contents are cooled down to between 0 and 5 degrees C
  3. temperatureis maintained between 0 and 5 degrees C
  4. customcondensed
  5. customThree fractions are collected
  6. customThe major (center) fraction from each injection is collected
  7. customcondensed

出典と根拠

ORDレコード
ord-64f7ad7374b14b85aca423a9c33a90bd
出典データセット
uspto-grants-1995_09
特許番号
US05449729

反応ノート

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