2,2,6,6-Tetramethylpiperidine → Piperidine, 1-chloro-2,2,6,6-tetramethyl-

HRID 1479701노트

반응식

HRID 1479701 반응식
[CH3:1][C:2]1([CH3:10])[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[NH:3]1.[OH-].[Ca+2].[OH-].[Cl:14]Cl>O>[Cl:14][N:3]1[C:4]([CH3:9])([CH3:8])[CH2:5][CH2:6][CH2:7][C:2]1([CH3:10])[CH3:1]

참가 물질

5

반응물 3

HCID 130352,2,6,6-TetramethylpiperidineHCID 24526Chlorine2회HCID 6093208Calcium Hydroxide

생성물 1

HCID 141712Piperidine, 1-chloro-2,2,6,6-tetramethyl-

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
5 °C

실험 절차

20 g of 2,2,6,6-tetramethylpiperidine are mixed with water and 6.42 g, 0.6 eq., of calcium hydroxide, and the suspension is cooled to 5° C. Over a period of 1.5 hours, 10.8 g, 1.1 eq. of chlorine gas are introduced, then nitrogen gas is used to drive out the excess chlorine and the mixture is warmed to RT. After separating the phases, washing the aqueous phase with 25 ml of dichloromethane, drying the combined organic phases with magnesium sulphate and distilling off the dichloromethane in vacuo, 24.2 g, 99%, of 1-chloro-2,2,6,6-tetramethylpiperidine are obtained.

후처리

  1. temperaturethe mixture is warmed to RT
  2. customAfter separating the phases
  3. washwashing the aqueous phase with 25 ml of dichloromethane
  4. dry with materialdrying the combined organic phases with magnesium sulphate
  5. distillationdistilling off the dichloromethane in vacuo, 24.2 g, 99%

출처 및 근거

ORD 기록
ord-6ba3ec8960bf4605bc06da9ac379ce66
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409863B2

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