Methyldichlorosilane → 3-(Dichloromethylsilyl)propyl 2-propenoate

HRID 637735

반응식

HRID 637735 반응식
[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]

참가 물질

5

반응물 2

HCID 6376Methyldichlorosilane2회HCID 13835Allyl acrylate

생성물 1

HCID 99645883-(Dichloromethylsilyl)propyl 2-propenoate수율 68.3%

시약·촉매·용매 2

HCID 7108Phenothiazine촉매2회HCID 11776Triphenylphosphine촉매

반응 조건

온도
65 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cbb47104230840fbb54142cd61d56e4c
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04558111

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