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Potassium Carbonate → 2-(4-Bromo-2-fluorophenyl)-1,2-thiazolidine-1,1-dione

HRID 858642
ノート
印刷プレビュー

反応式

HRID 858642 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][S:9]([CH2:12][CH2:13][CH2:14]Cl)(=[O:11])=[O:10])=[C:4]([F:16])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][S:9]2(=[O:11])=[O:10])=[C:4]([F:16])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 43654020N-(4-bromo-2-fluorophenyl)-3-chloropropane-1-sulfonamide

生成物 1

HCID 246946312-(4-Bromo-2-fluorophenyl)-1,2-thiazolidine-1,1-dione収率 122.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-(4-bromo-2-fluorophenyl)-3-chloropropane-1-sulfonamide (8.27 g, 0.025M) and potassium carbonate (5.10 g, 0.0375M) was dissolved in dimethylformamide (50 ml) at room temperature under an atmosphere of nitrogen. The reaction mixture was stirred for a further 24 hrs after which time it was partitioned between diethylether (500 ml) and water (500 ml). The organics were washed with 1N HCl (300 ml) and then water (100 ml) The organics were then dried over magnesium sulfate, filtered and the solvent concentrated in vacuuo to afford the title compound as a brown oil (9.0 g). 1H NMR (CDCl3): δ 2.40–2.50 (m, 2H), 3.25–3.40 (m, 2H), 4.00 (m, 2H); 6.78 (m, 2H), 7.10 (d, J=2.56 Hz, 1H),).

後処理

  1. customwas partitioned between diethylether (500 ml) and water (500 ml)
  2. washThe organics were washed with 1N HCl (300 ml)
  3. dry with materialwater (100 ml) The organics were then dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe solvent concentrated in vacuuo

出典と根拠

ORDレコード
ord-cacfa1475fde4d61b75b776c2bf59f37
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07148226B2

反応ノート

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