Potassium Carbonate → 4-{[(4-Chloro-benzenesulfonyl)-(5-isopropyl-2-oxo-azepan-3-yl)-amino]-methyl}-benzamide

HRID 851981ノート

反応式

HRID 851981 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][CH:12]2[CH2:18][CH:17]([CH:19]([CH3:21])[CH3:20])[CH2:16][CH2:15][NH:14][C:13]2=[O:22])(=[O:10])=[O:9])=[CH:4][CH:3]=1.Br[C:24]1[CH:32]=[CH:31][C:27]([C:28]([NH2:30])=[O:29])=[C:26](C)[CH:25]=1.[C:34]([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([N:11]([CH2:34][C:24]2[CH:25]=[CH:26][C:27]([C:28]([NH2:30])=[O:29])=[CH:31][CH:32]=2)[CH:12]2[CH2:18][CH:17]([CH:19]([CH3:20])[CH3:21])[CH2:16][CH2:15][NH:14][C:13]2=[O:22])(=[O:10])=[O:9])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 206167664-Bromo-2-methylbenzamideHCID 694892534-Chloro-N-(5-isopropyl-2-oxo-azepan-3-yl)-benzenesulfonamide

生成物 1

HCID 116559084-{[(4-Chloro-benzenesulfonyl)-(5-isopropyl-2-oxo-azepan-3-yl)-amino]-methyl}-benzamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
65 °C

実験手順

4-Chloro-N-(5-isopropyl-2-oxo-azepan-3-yl)-benzenesulfonamide (0.06 g, 0.17 mmol), 4-bromo-methyl-benzamide (0.06 g, 0.25 mmol), K2CO3 (0.24 g, 1.7 mmol), KI (0.01 g, 0.06 mmol) were added to dry DMF (5 ml) and the resultant reaction mixture was shaken overnight at 65° C. under an argon atmosphere. The solvent was removed under reduced pressure and the residue taken up in ethyl acetate and washed with 5% KHSO4/10% K2SO4 (2×), water, brine, dried (MgSO4), filtered, concentrated under reduced pressure and purified using preparative RP(C18) chromatography: lyophilisate 23 mg; MS: m/e=478.3 (MH+), 495.4 (MNH4+)

後処理

  1. customthe resultant reaction mixture
  2. customThe solvent was removed under reduced pressure
  3. washwashed with 5% KHSO4/10% K2SO4 (2×), water, brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. custompurified

出典と根拠

ORDレコード
ord-7b475eeaec1b4a0cbd8a0514248b3189
出典データセット
uspto-grants-2007_08
特許番号
US07253158B2

反応ノート

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