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Potassium Carbonate → HCID 11123863、化合物

HRID 991111
ノート
印刷プレビュー

反応式

HRID 991111 の反応式
Cl.Cl[CH2:3][CH2:4][N:5]([CH2:13][CH2:14]Cl)[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C1OCCOCCOCCOCCOCCOC1.C([O-])([O-])=O.[K+].[K+].[CH2:40]([O:42][C:43](=[O:62])[CH2:44][S:45]([C:48]1[CH:53]=[CH:52][C:51]([O:54][CH2:55][C:56]2[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=2)=[CH:50][CH:49]=1)(=[O:47])=[O:46])[CH3:41]>CC(C)=O>[CH2:40]([O:42][C:43]([C:44]1([S:45]([C:48]2[CH:53]=[CH:52][C:51]([O:54][CH2:55][C:56]3[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=3)=[CH:50][CH:49]=2)(=[O:47])=[O:46])[CH2:14][CH2:13][N:5]([CH2:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH2:4][CH2:3]1)=[O:62])[CH3:41]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 2777881N,N-Bis(2-chloroethyl)benzylamine hydrochlorideHCID 10947619(4-Benzyloxy-phenylsulfonyl)-acetic acid ethyl ester

生成物 1

HCID 11123863HCID 11123863、化合物

試薬・触媒・溶媒 1

HCID 180Acetone
溶媒

実験手順

To a stirred solution of bis-(2-chloro-ethyl)-benzyl amine hydrochloride (6.6 g, 24.7 mmol), 18-Crown-6 (500 mg), and anhydrous K2CO3 (30 gm, excess) in dry acetone (250 ml), (4- benzyloxy-phenylsulfonyl)-acetic acid ethyl ester (8.01 gm, 24 mmol) was added in a round bottom flask and the reaction mLxture was heated at reflux for 16 hours with good stirring. At the end, the reaction mixture was allowed to cool and the potassium salts were filtered off and the reaction mixture was concentrated. The residue was extracted with chloroform and washed with H2O . The organic layer was further washed well with water, dried over MgSO4, filtered and concentrated. The dark brown reaction mixture was purified by silica gel coumn chromatography by eluting it with 30% ethylacetate: hexane and the product 4-(4-Benzyloxy-benzenesulfonyl)-1-benzyl-piperidine-4-carboxylic acid ethyl ester was isolated as Brown oil. Yield: 6.5 g, 55%; MS: 494 (M+H)

後処理

  1. temperaturethe reaction mLxture was heated
  2. temperatureat reflux for 16 hours with good stirring
  3. temperatureto cool
  4. filtrationthe potassium salts were filtered off
  5. concentrationthe reaction mixture was concentrated
  6. extractionThe residue was extracted with chloroform
  7. washwashed with H2O
  8. washThe organic layer was further washed well with water
  9. dry with materialdried over MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customThe dark brown reaction mixture was purified by silica gel coumn chromatography
  13. washby eluting it with 30% ethylacetate

出典と根拠

ORDレコード
ord-6f7d6662e1c341df956f92a0ae093fc8
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06462073B2

反応ノート

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