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

HRID 1479701ノート

反応式

HRID 1479701 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-].[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]

参加物

5

反応物 3

HCID 130352,2,6,6-TetramethylpiperidineHCID 24526Chlorine2 回HCID 6093208Calcium Hydroxide

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

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.

後処理

  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%

出典と根拠

ORDレコード
ord-6ba3ec8960bf4605bc06da9ac379ce66
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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