Potassium Carbonate → HCID 19003511、化合物

HRID 2259408ノート

反応式

HRID 2259408 の反応式
[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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 11636816N,N-Dimethylaminoethyl chloride hydrochlorideHCID 53400706HCID 53400706、化合物

生成物 1

HCID 19003511HCID 19003511、化合物収率 64.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a73c1ec75485464f9cbdd007ed6a02cf
出典データセット
uspto-grants-1995_12
特許番号
US05473066

反応ノート

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