2,2,7,7-Tetramethyl-3,6-dioxa-2,7-disilaoctane → HCID 14638051, 화합물

HRID 521302

반응식

HRID 521302 반응식
C[Si](C)(C)[O:3][CH2:4][CH2:5][O:6][Si](C)(C)C.[CH3:13][C:14]([CH3:23])([CH2:19][N+:20]([O-:22])=[O:21])[CH2:15][C:16](=O)[CH3:17]>ClCCl.FC(F)(F)S(O[Si](C)(C)C)(=O)=O>[CH3:13][C:14]([CH3:23])([CH2:19][N+:20]([O-:22])=[O:21])[CH2:15][C:16]1([CH3:17])[O:6][CH2:5][CH2:4][O:3]1

참가 물질

5

반응물 2

HCID 818582,2,7,7-Tetramethyl-3,6-dioxa-2,7-disilaoctaneHCID 41563834,4-Dimethyl-5-nitropentan-2-one

생성물 1

HCID 14638051HCID 14638051, 화합물수율 97.2%

시약·촉매·용매 2

HCID 65367Trimethylsilyl triflate촉매HCID 6344Dichloromethane용매2회

실험 절차

A stirred solution of 1,2-bis(trimethylsilyloxy)ethane (26.5 g, 128 mmol) in dichloromethane (50 mL) was cooled in a dry ice/isopropanol bath, and trimethylsilyl trifluoromethanesulfonate (2.2 g, 1.0 mmol) was added, followed by the dichloromethane solution of 4,4-dimethyl-5-nitropentan-2-one (50 mL, 19.0 g, 119 mmol) from the previous step. After 30 minutes, the cooling bath was removed and the solution was allowed to warm to room temperature. The solution was filtered through a plug of potassium carbonate and concentrated under reduced pressure to provide 2-(2,2-dimethyl-3-nitropropyl)-2-methyl-[1,3]dioxolane (23.5 g) as a dark oil that was used directly in the next step without further purification.

후처리

  1. customthe cooling bath was removed
  2. filtrationThe solution was filtered through a plug of potassium carbonate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-cc8b8aaf51d44583aafc7dd54d21a15e
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09328110B2

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