Potassium Carbonate → HCID 19003511, 화합물

HRID 2259408노트

반응식

HRID 2259408 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[CH:7][S:8](=O)[C:4]=2[CH:3]=1.Cl.[CH3:13][N:14]([CH2:16][CH2:17]Cl)[CH3:15].C([O-])([O-])=[O:20].[K+].[K+]>CC(C)=O>[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]([CH2:17][CH2:16][N:14]([CH3:15])[CH3:13])[C:7](=[O:20])[S:8][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 11636816N,N-Dimethylaminoethyl chloride hydrochlorideHCID 53400706HCID 53400706, 화합물

생성물 1

HCID 19003511HCID 19003511, 화합물수율 64.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of compound (VIII) (9.28 g, 50 mmol), N,N-dimethylaminoethylchloride hydrochloride (XIe) (7.92 g, 55 mmol), and K2CO3 (16.58 g, 120 mmol) in acetone (93 ml) was refluxed for 20 hours with stirring. After the reaction was complete, the reaction mixture was concentrated in vacuo. The residue was extracted with ethyl acetate. The layer of ethyl acetate was dried over MgSO4 and subjected to column chromatography on silica gel. From the eluate eluted with ethyl acetate, compound (XIIe) (3.3 g, yield=64.3%) was obtained as an oil.

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. extractionThe residue was extracted with ethyl acetate
  3. dry with materialThe layer of ethyl acetate was dried over MgSO4
  4. washFrom the eluate eluted with ethyl acetate
  5. customcompound (XIIe) (3.3 g, yield=64.3%) was obtained as an oil

출처 및 근거

ORD 기록
ord-a73c1ec75485464f9cbdd007ed6a02cf
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05473066

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