Chlorotrimethylsilane → HCID 56624785, 화합물

HRID 464559노트

반응식

HRID 464559 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-dichloroacetyl-piperid-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 gravity 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 gravity 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-25e7228a48be47aabd12875722ee9fcf
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04548639

반응 노트

불러오는 중…