Benzenesulfonyl chloride → HCID 22033525、化合物

HRID 325034ノート

反応式

HRID 325034 の反応式
[C:1]1([S:7](Cl)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH2:19][CH2:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]#[N:28])=[CH:23][CH:22]=2)[C:13]=1[CH3:29]>N1C=CC=CC=1>[C:27]([C:24]1[CH:25]=[CH:26][C:21]([CH2:20][CH2:19][O:18][C:14]2[C:13]([CH3:29])=[C:12]([NH:11][S:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)(=[O:9])=[O:8])[CH:17]=[CH:16][CH:15]=2)=[CH:22][CH:23]=1)#[N:28]

参加物

4

反応物 2

HCID 7369Benzenesulfonyl chlorideHCID 22033540Amino-3-[2-(4-cyanophenyl)ethoxy]-2-methylbenzene

生成物 1

HCID 22033525HCID 22033525、化合物収率 72%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Benzenesulfonyl chloride (0.24 mL; 1.9 mmol) was added to a stirred solution of amino-3-[2-(4-cyanophenyl)ethoxy]-2-methylbenzene (0.42 g; 1.7 mmol; from step (iii) above) in dry pyridine (20 mL) under nitrogen. The reaction was left overnight at room temperature. After evaporation of the solvent the residue was partitioned between 10% aqueous HCl and EtOAc. The organic layer was washed with brine, dried (MgSO4) and the solvent removed in vacuo. Purification by flash chromatography afforded 0.47 g (72%) of the sub-title compound.

後処理

  1. customAfter evaporation of the solvent the residue
  2. customwas partitioned between 10% aqueous HCl and EtOAc
  3. washThe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed in vacuo
  6. customPurification by flash chromatography

出典と根拠

ORDレコード
ord-e0db434525a843a8b594c247d886eb75
出典データセット
uspto-grants-2001_04
特許番号
US06221898B1

反応ノート

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