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1,2-Dichloroethane → 4-Chloro-N-(4-pentyl-bicyclo[2.2.2]octane-1-carbonyl)-benzenesulfonamide

HRID 1455546
ノート
印刷プレビュー

反応式

HRID 1455546 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(Cl)CCl.[CH2:16]([C:21]12[CH2:28][CH2:27][C:24]([C:29](O)=[O:30])([CH2:25][CH2:26]1)[CH2:23][CH2:22]2)[CH2:17][CH2:18][CH2:19][CH3:20]>CN(C1C=CN=CC=1)C.CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([NH:11][C:29]([C:24]23[CH2:25][CH2:26][C:21]([CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])([CH2:28][CH2:27]2)[CH2:22][CH2:23]3)=[O:30])(=[O:9])=[O:10])=[CH:6][CH:7]=1
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 3

HCID 111,2-DichloroethaneHCID 668244-ChlorobenzenesulfonamideHCID 42414664-Pentylbicyclo[2.2.2]octane-1-carboxylic acid

生成物 1

HCID 684417734-Chloro-N-(4-pentyl-bicyclo[2.2.2]octane-1-carbonyl)-benzenesulfonamide

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 6228
Dimethylformamide
溶媒

実験手順

0.42 g of 4-chlorophenylsulfonamide, 60 mg of DMAP and 0.42 g of EDC are added to a solution of 0.5 g of 4-pentyl-bicyclo[2.2.2]octane-1-carboxylic acid in 8 ml of DMF, the mixture obtained is stirred for ca. 16 h at RT and solvent from the mixture obtained is evaporated. The evaporation residue obtained is dissolved in EtAc and washed with 1 N HCl, saturated NaHCO3 solution and brine and the organic phase obtained is dried. Solvent of the organic phase obtained is evaporated and the evaporation residue obtained is subjected to chromatography. 4-Chloro-N-(4-pentyl- bicyclo[2.2.2]octane-1-carbonyl)-benzenesulfonamide is obtained in the form of a white powder;

後処理

  1. customthe mixture obtained
  2. customsolvent from the mixture obtained
  3. customis evaporated
  4. customThe evaporation residue obtained
  5. dissolutionis dissolved in EtAc
  6. washwashed with 1 N HCl, saturated NaHCO3 solution and brine
  7. customthe organic phase obtained
  8. customis dried
  9. customSolvent of the organic phase obtained
  10. customis evaporated
  11. customthe evaporation residue obtained

出典と根拠

ORDレコード
ord-356bd4791c184ed6818a06a875ebc721
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482462B2

反応ノート

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