Propane sultone → 1-propanaminium, n,n-dimethyl-n-(3-((2-methyl-1-oxo-2-propen-1-yl)amino)propyl)-3-sulfo-, inner salt

HRID 1504108

反応式

HRID 1504108 の反応式
[CH2:1]1[S:5](=[O:7])(=[O:6])[O:4][CH2:3][CH2:2]1.[CH3:8][C:9]([C:11]([NH:13][CH2:14][CH2:15][CH2:16][N:17]([CH3:19])[CH3:18])=[O:12])=[CH2:10]>C(#N)C>[C:11]([NH:13][CH2:14][CH2:15][CH2:16][N+:17]([CH3:19])([CH3:18])[CH2:3][CH2:2][CH2:1][S:5]([O-:4])(=[O:7])=[O:6])(=[O:12])[C:9]([CH3:10])=[CH2:8]

参加物

4

反応物 2

HCID 14264Propane sultoneHCID 78882N-(3-(Dimethylamino)propyl)methacrylamide

生成物 1

HCID 788831-propanaminium, n,n-dimethyl-n-(3-((2-methyl-1-oxo-2-propen-1-yl)amino)propyl)-3-sulfo-, inner salt

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

反応条件

温度
35 °C

実験手順

Into a round bottom flask is added 26.4 grams of anhydrous acetonitrile (available from Sigma-Aldrich) and 15.5 grams of propane sultone (available from Sigma-Aldrich), and this is stirred for 30 minutes. After the 30 minutes, a solution of 25.6 grams of DMAPMA in 56.5 grams of acetonitrile is added. The mixture is stirred and warmed to 35° C. A white precipitate quickly forms. Once the white precipitate takes up the bulk of the volume, the liquid is decanted. The solid is washed once with acetonitrile and again the liquid is removed by decanting. The solids are then washed in 2× volume diethyl ether. They are then filtered via funnel and washed with copious amounts (via filtration) of diethyl ether. The NMR structure is consistent with the structure of the target molecule SZ.

後処理

  1. stirringThe mixture is stirred
  2. customthe liquid is decanted
  3. washThe solid is washed once with acetonitrile
  4. customagain the liquid is removed
  5. customby decanting
  6. washThe solids are then washed in 2× volume diethyl ether
  7. filtrationThey are then filtered via funnel
  8. washwashed with copious amounts (via filtration) of diethyl ether

出典と根拠

ORDレコード
ord-8b3c647cc42a4ddbbeabd80c2a6f960b
出典データセット
uspto-grants-2015_12
特許番号
US09212243B2

関連ノート

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