Hydrochloric Acid → 3-chloro-N,N-dimethylpropane-1-sulfonamide

HRID 890244ノート

反応式

HRID 890244 の反応式
Cl.[CH3:2][NH:3][CH3:4].[Cl:5][CH2:6][CH2:7][CH2:8][S:9](Cl)(=[O:11])=[O:10].[OH-].[Na+].Cl>O>[Cl:5][CH2:6][CH2:7][CH2:8][S:9]([N:3]([CH3:4])[CH3:2])(=[O:11])=[O:10]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10473Dimethylamine, hydrochlorideHCID 14798Sodium HydroxideHCID 154103-Chloropropanesulphonyl chloride

生成物 1

HCID 100353283-chloro-N,N-dimethylpropane-1-sulfonamide

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
-5 °C

実験手順

10 g of dimethylamine hydrochloride are placed in 60 ml of water, a nitrogen atmosphere is applied and the solution is cooled to between 0° C. and −5° C., and then 18 ml of 3-chloro-1-propanesulphonyl chloride are added dropwise. 10.6 g of sodium hydroxide in 40 ml of water are added while maintaining at −5° C., then the mixture is allowed to return to AT and stirring is maintained for 1 hour. 1 ml of concentrated HCl is added and then extraction is carried out with DCM. The organic phase is washed with a 10% NaOH solution and then with an NaCl solution. 15.1 g of the expected compound are obtained.

後処理

  1. temperaturethe solution is cooled to between 0° C. and −5° C.
  2. temperatureis maintained for 1 hour
  3. extractionextraction
  4. washThe organic phase is washed with a 10% NaOH solution

出典と根拠

ORDレコード
ord-36fd1e0ba7ea4cacb7cd98a20ef9e7d7
出典データセット
uspto-grants-2006_02
特許番号
US06995184B2

反応ノート

読み込み中…