Hydrochloric Acid → N-(3,5-Difluoro-4-iodopyridin-2-yl)propane-1-sulfonamide

HRID 710572ノート

反応式

HRID 710572 の反応式
[F:1][C:2]1[C:3]([N:10](S(CCC)(=O)=O)[S:11]([CH2:14][CH2:15][CH3:16])(=[O:13])=[O:12])=[N:4][CH:5]=[C:6]([F:9])[C:7]=1[I:8].Cl>[OH-].[Na+]>[F:1][C:2]1[C:3]([NH:10][S:11]([CH2:14][CH2:15][CH3:16])(=[O:13])=[O:12])=[N:4][CH:5]=[C:6]([F:9])[C:7]=1[I:8]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67366767N-(3,5-Difluoro-4-iodopyridin-2-yl)-N-(propylsulfonyl)propane-1-sulfonamide

生成物 1

HCID 86686187N-(3,5-Difluoro-4-iodopyridin-2-yl)propane-1-sulfonamide

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

Crude N-(3,5-Difluoro-4-iodopyridin-2-yl)-N-(propylsulfonyl)propane-1-sulfonamide (obtained in Step 1) was stirred with 5% aqueous sodium hydroxide solution (20 ml) at 60° C. for 1 h. The cooled reaction mixture was then acidified with 10% hydrochloric acid to pH<2 and extracted with DCM. The combined extracts were dried over sodium sulfate, filtered, and concentrated. The residue was chromatographed on silica gel (20-30% ethyl acetate in hexanes eluant) to provide the title compound. MS m/z 363.1 (M+1).

後処理

  1. customThe cooled reaction mixture
  2. extractionextracted with DCM
  3. dry with materialThe combined extracts were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel (20-30% ethyl acetate in hexanes eluant)

出典と根拠

ORDレコード
ord-07c72adc46f04d1a829582da38132b7b
出典データセット
uspto-grants-2015_11
特許番号
US09181238B2

反応ノート

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