Diethyl Ether → HCID 11984250, 화합물

HRID 496977

반응식

HRID 496977 반응식
Cl.[C:2]([O:7][CH2:8][CH2:9][NH2:10])(=[O:6])[C:3]([CH3:5])=[CH2:4].C(N(CC)CC)C.[F:18][C:19]([F:25])([F:24])[S:20](Cl)(=[O:22])=[O:21].CCOCC>C(Cl)Cl>[C:2]([O:7][CH2:8][CH2:9][NH:10][S:20]([C:19]([F:25])([F:24])[F:18])(=[O:22])=[O:21])(=[O:6])[C:3]([CH3:5])=[CH2:4]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 75495Aminoethyl methacrylate hydrochlorideHCID 79000Trifluoromethanesulfonyl chloride

생성물 1

HCID 11984250HCID 11984250, 화합물수율 61%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 15 g (0.091 mol) of 2-aminoethyl methacrylate hydrochloride (available from Aldrich) in 250 ml of anhydrous methylene chloride was added 18.4 g of redistilled triethylamine (0.182 mol). After the mixture was stirred at room temperature for 1 hour, 15.3 g trifluoromethane sulfonylchloride (0.091 mol) was added. The resulting mixture was further stirred at room temperature overnight. About 200 ml ether was added. The mixture was filtered to remove the precipitate formed. The filtrate was sequentially washed with 2×100 ml of 5% HCl, 100 ml of saturated NaHCO3, 2×100 ml brine, and then dried over MgSO4. The solvents were removed by rotavap. About 14.5 g of viscous liquid was obtained. The product was further purified by recrystallization from 1:1 hexane/chloroform to give about 12 g white solid (51%) having a melting point of 55-58° C.

후처리

  1. stirringThe resulting mixture was further stirred at room temperature overnight
  2. filtrationThe mixture was filtered
  3. customto remove the precipitate
  4. customformed
  5. washThe filtrate was sequentially washed with 2×100 ml of 5% HCl, 100 ml of saturated NaHCO3, 2×100 ml brine
  6. dry with materialdried over MgSO4
  7. customThe solvents were removed by rotavap

출처 및 근거

ORD 기록
ord-89ca2ed0925549bc827c6456d93adc7d
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949325B2

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