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

HRID 1479700노트

반응식

HRID 1479700 반응식
[CH3:1][C:2]1([CH3:10])[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[NH:3]1.[OH-].[Na+].[Cl:13]Cl>>[Cl:13][N:3]1[C:4]([CH3:9])([CH3:8])[CH2:5][CH2:6][CH2:7][C:2]1([CH3:10])[CH3:1]

참가 물질

4

반응물 3

HCID 130352,2,6,6-TetramethylpiperidineHCID 14798Sodium HydroxideHCID 24526Chlorine2회

생성물 1

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

반응 조건

온도
7.5 °C

실험 절차

20 g of 2,2,6,6-tetramethylpiperidine are mixed with 40.7 g, 1.1 eq, of 15% sodium hydroxide solution and cooled to 5 to 10° 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 room temperature (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 room temperature (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-38bd88183b6749e990adb0de892e03ae
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409863B2

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