Cesium carbonate → HCID 66895718、化合物

HRID 633133ノート

反応式

HRID 633133 の反応式
Br[CH2:2][CH2:3][N:4]1[CH:8]=[CH:7][CH:6]=[CH:5]1.C(=O)([O-])[O-].[Cs+].[Cs+].[Cl:15][C:16]1[CH:25]=[C:24]([NH:26][S:27]([CH3:30])(=[O:29])=[O:28])[CH:23]=[CH:22][C:17]=1[C:18]([O:20][CH3:21])=[O:19]>CN(C=O)C>[N:4]1([CH2:3][CH2:2][N:26]([C:24]2[CH:23]=[CH:22][C:17]([C:18]([O:20][CH3:21])=[O:19])=[C:16]([Cl:15])[CH:25]=2)[S:27]([CH3:30])(=[O:28])=[O:29])[CH:8]=[CH:7][CH:6]=[CH:5]1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 116512251-(2-Bromoethyl)pyrroleHCID 54238017Methyl 2-chloro-4-(methylsulfonamido)benzoate

生成物 1

HCID 66895718HCID 66895718、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

200 μL of 1-(2-bromoethyl)-1H-pyrrole and 556 mg of Cesium Carbonate were added to 150 mg of methyl 2-chloro-4-(methylsulfonamido)benzoate in DMF and stirred at room temperature for 16 hours. The reaction mixture was extracted in Ethyl Acetate twice with saturated bicarbonate and once with brine, dried over Magnesium Sulfate, filtered and concentrated to give methyl 4-(N-(2-(1H-pyrrol-1-yl)ethyl)methylsulfonamido)-2-chlorobenzoate. 230 mg of methyl 4-(N-(2-(1H-pyrrol-1-yl)ethyl)methylsulfonamido)-2-chlorobenzoate was hydrolyzed via Procedure M to yield 221 mg of crude 4-(N-(2-(1H-pyrrol-1-yl)ethyl)methylsulfonamido)-2-chlorobenzoic acid.

後処理

  1. extractionThe reaction mixture was extracted in Ethyl Acetate twice with saturated bicarbonate and once with brine
  2. dry with materialdried over Magnesium Sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-1972b8779599417bb4edb2eef7fe9110
出典データセット
uspto-grants-2016_04
特許番号
US09321761B2

反応ノート

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