Methyldichlorosilane → 3-(Dichloromethylsilyl)propyl 2-propenoate

HRID 637735

反応式

HRID 637735 の反応式
[CH2:1]([O:4][C:5](=[O:8])[CH:6]=[CH2:7])[CH:2]=[CH2:3].[CH3:9][SiH:10]([Cl:12])[Cl:11]>C1C2NC3C(=CC=CC=3)SC=2C=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[C:5]([O:4][CH2:1][CH2:2][CH2:3][Si:10]([CH3:9])([Cl:12])[Cl:11])(=[O:8])[CH:6]=[CH2:7]

参加物

5

反応物 2

HCID 6376Methyldichlorosilane2 回HCID 13835Allyl acrylate

生成物 1

HCID 99645883-(Dichloromethylsilyl)propyl 2-propenoate収率 68.3%

試薬・触媒・溶媒 2

HCID 7108Phenothiazine触媒2 回HCID 11776Triphenylphosphine触媒

反応条件

温度
65 °C

実験手順

To a three-necked flask equipped as in Example 1 there was added 260 grams allylacrylate (2.32 moles), 0.5 grams catalyst prepared in accordance with U.S. Pat. No. 3,814,730 (2.6 weight percent Pt) and 1.04 grams phenothiazine. The mixture was heated with stirring to 65° C. and, using the vent of the condenser, purged with nitrogen. The heat source was then turned off and 237 grams (2.32 moles) CH3SiHCl2 was added dropwise, the temperature of the reaction mass being maintained at about 70° C. Upon completion of the addition of methyldichlorosilane the crude product was cooled to room temperature. One gram phenothiazine and 0.05 gram triphenyl phosphine were added to the product prior to distillation. Acryloxypropylmethyldichlorosilane (360 grams, 68% yield) was distilled at 109°-112° C./10 mm Hg.

後処理

  1. customTo a three-necked flask equipped as in Example 1 there
  2. customprepared in accordance with U.S
  3. temperatureThe mixture was heated
  4. custompurged with nitrogen
  5. temperaturethe temperature of the reaction mass being maintained at about 70° C
  6. temperaturewas cooled to room temperature
  7. distillationto distillation

出典と根拠

ORDレコード
ord-cbb47104230840fbb54142cd61d56e4c
出典データセット
uspto-grants-1985_12
特許番号
US04558111

関連ノート

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