2,2,7,7-Tetramethyl-3,6-dioxa-2,7-disilaoctane → HCID 14638051、化合物

HRID 521302

反応式

HRID 521302 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 14638051HCID 14638051、化合物収率 97.2%

試薬・触媒・溶媒 2

HCID 65367Trimethylsilyl triflate触媒HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-cc8b8aaf51d44583aafc7dd54d21a15e
出典データセット
uspto-grants-2016_05
特許番号
US09328110B2

関連ノート

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