Chlorotrimethylsilane → HCID 56624785, 화합물

HRID 65388노트

반응식

HRID 65388 반응식
[Cl:1][CH:2]([Cl:12])[C:3]([N:5]1[CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]1)=[O:4].[CH2:13](O)[CH2:14][CH2:15][OH:16].C[Si](C)(C)Cl>>[CH2:15]1[O:16][C:8]2([CH2:7][CH2:6][N:5]([C:3](=[O:4])[CH:2]([Cl:1])[Cl:12])[CH2:10][CH2:9]2)[O:11][CH:14]1[CH3:13]

참가 물질

4

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 104421,3-PropanediolHCID 130182281-(Dichloroacetyl)piperidin-4-one

생성물 1

HCID 56624785HCID 56624785, 화합물수율 66.6%

실험 절차

A mixture of 19 g (0.09 mol) of N-dichloroacetylpiperid-4-one, 7.5 g (0.099 mol) of propane-1,3-diol and 22.4 g (0.21 mol) of trimethylchlorosilane was boiled under reflux for 12 hours, while stirring. Thereafter, the reaction mixture was concentrated under reduced pressure and the residue was then subjected to brief incipient distillation under greatly reduced pressure. The resulting brown oil, which slowly crystallized completely, was recrystallized from 200 ml of toluene. 16 g (66.6% of theory) of N-dichloroacetyl-piperid-4-one propylene ketal of melting point 115° C. were obtained.

후처리

  1. temperatureunder reflux for 12 hours
  2. concentrationThereafter, the reaction mixture was concentrated under reduced pressure
  3. distillationthe residue was then subjected to brief incipient distillation under greatly reduced pressure
  4. customThe resulting brown oil, which slowly crystallized completely
  5. customwas recrystallized from 200 ml of toluene

출처 및 근거

ORD 기록
ord-39fcff8cd157445eaa6313081d773d75
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614537

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