Hydrochloric Acid → Dimethyl(1-octenyl)(2-pyridyl)silane

HRID 1860981

반응식

HRID 1860981 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH:20]#[C:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27].[CH3:28][SiH:29]([CH3:36])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][N:31]=1.Cl>C(OCC)C>[CH3:28][Si:29]([CH3:36])([CH:20]=[CH:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][N:31]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 123701-OctyneHCID 91999694HCID 91999694, 화합물

생성물 1

HCID 53632469Dimethyl(1-octenyl)(2-pyridyl)silane수율 90.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
40 °C

실험 절차

To 1.0 ml of diethyl ether were added 10 mg (0.25 μmol) of bis(cyclooctadiene)platinum, 13 mg (0.50 μmol) of triphenylphosphine and 165 mg (1.5 mmol) of 1-octyne, and 69 mg (0.5 mmol) of dimethyl(2-pyridyl)silane was added dropwise thereto at room temperature over 1 hour. Further, the mixture was continued to be stirred for 6 hours at an inner temperature of 40° C., followed by the addition of 6 ml of 1N hydrochloric acid and 5 ml of diethyl ether. After the mixture was stirred for 30 minutes, it was left stand and separated into the organic and aqueous layers. The organic layer was extracted with five portions of 6 ml of 1N hydrochloric acid, and the resulting aqueous layers were combined together and turned basic with the addition of sodium hydroxide pellets. This aqueous layer was extracted with three portions of 10 ml of diethyl ether. The resulting organic layer was dried over magnesium sulfate and the solvent was evaporated off under reduced pressure to give 112 mg of dimethyl(1-octenyl)(2-pyridyl)silane. Yield: 90%

후처리

  1. additionwas added dropwise
  2. stirringAfter the mixture was stirred for 30 minutes
  3. waitit was left stand
  4. customseparated into the organic and aqueous layers
  5. extractionThe organic layer was extracted with five portions of 6 ml of 1N hydrochloric acid
  6. additionturned basic with the addition of sodium hydroxide pellets
  7. extractionThis aqueous layer was extracted with three portions of 10 ml of diethyl ether
  8. dry with materialThe resulting organic layer was dried over magnesium sulfate
  9. customthe solvent was evaporated off under reduced pressure

출처 및 근거

ORD 기록
ord-97440b84bd7f482ea5d3857fe985a647
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06531602B2

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