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

HRID 1479700ノート

反応式

HRID 1479700 の反応式
[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]

参加物

4

反応物 3

HCID 130352,2,6,6-TetramethylpiperidineHCID 14798Sodium HydroxideHCID 24526Chlorine2 回

生成物 1

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

反応条件

温度
7.5 °C

実験手順

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.

後処理

  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%

出典と根拠

ORDレコード
ord-38bd88183b6749e990adb0de892e03ae
出典データセット
uspto-grants-2016_08
特許番号
US09409863B2

反応ノート

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