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

HRID 532071

반응식

HRID 532071 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

반응 조건

온도
35 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-18fa32194ced452b8ae9a8e971c8a541
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08852399B2

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