Sodium Bicarbonate → HCID 23114571、化合物

HRID 2080484ノート

反応式

HRID 2080484 の反応式
[Cl:1][C:2]1[C:3]([CH:20]([C:31]2[CH:36]=[C:35]([F:37])[CH:34]=[CH:33][C:32]=2[F:38])[S:21]([C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)(=[O:23])=[O:22])=[CH:4][C:5]([NH:8]CC2C=CC(OC)=C(OC)C=2)=[N:6][CH:7]=1.C(=O)(O)[O-].[Na+]>FC(F)(F)C(O)=O>[Cl:1][C:2]1[C:3]([CH:20]([C:31]2[CH:36]=[C:35]([F:37])[CH:34]=[CH:33][C:32]=2[F:38])[S:21]([C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)(=[O:23])=[O:22])=[CH:4][C:5]([NH2:8])=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 23114881HCID 23114881、化合物

生成物 1

HCID 23114571HCID 23114571、化合物収率 99%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
65 °C

実験手順

[5-Chloro-4-[(2,5-difluorophenyl)-(4-fluorophenylsulfonyl)methyl]pyridin-2-yl](3,4-dimethoxybenzyl)amine (157 mg, 0.28 mmol) was dissolved in trifluoroacetic acid (5.0 ml). The resulting solution was stirred at 65° C. for 17 hours. After cooling, the reaction mixture was concentrated under reduced pressure. To the residue thus obtained was added a saturated aqueous solution of sodium bicarbonate. The resulting mixture was extracted with ethyl acetate. The extract was washed with brine, dried and concentrated under reduced pressure. The residue thus obtained was purified by silica gel chromatography (hexane:ethyl acetate=3:1) to give the title compound (114 mg, 99%) as a white solid.

後処理

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customTo the residue thus obtained
  4. extractionThe resulting mixture was extracted with ethyl acetate
  5. washThe extract was washed with brine
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customThe residue thus obtained
  9. customwas purified by silica gel chromatography (hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-5f750d910f4d431db5caa9b892e6826c
出典データセット
uspto-grants-2011_04
特許番号
US07932271B2

反応ノート

読み込み中…