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

HRID 710572노트

반응식

HRID 710572 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-07c72adc46f04d1a829582da38132b7b
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181238B2

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