Hydrochloric Acid → N-[4-(aminomethyl)-2,6-difluorophenyl]methanesulfonamide hydrochloride

HRID 1350851노트

반응식

HRID 1350851 반응식
[C:1]([C:3]1[CH:8]=[C:7]([F:9])[C:6]([NH:10][S:11]([CH3:14])(=[O:13])=[O:12])=[C:5]([F:15])[CH:4]=1)#[N:2].[ClH:16]>CO.O1CCCC1.[C].[Pd]>[ClH:16].[NH2:2][CH2:1][C:3]1[CH:4]=[C:5]([F:15])[C:6]([NH:10][S:11]([CH3:14])(=[O:13])=[O:12])=[C:7]([F:9])[CH:8]=1

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 21097536N-(4-cyano-2,6-difluorophenyl)methanesulfonamide

생성물 1

HCID 21097523N-[4-(aminomethyl)-2,6-difluorophenyl]methanesulfonamide hydrochloride수율 80%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of N-(4-cyano-2,6-difluorophenyl)methanesulfonamide (1.01 g, 4.35 mmol) in methanol (15 ml), tetrahydrofuran (15 ml) and 12 M aqueous solution of hydrogen chloride (5 ml) was hydrogenated over 10% palladium-carbon (250 mg) under ballon pressure for 3 h at ambient temperature. The catalyst was filtered through a pad of celite and the filter cake was washed with methanol. After the filtrate and washings were evaporated in vacuo, the residue was recrystallized from methanol and diisopropyl ether to give to furnish 953 mg (80% yield) of the title compound as a white solid.

후처리

  1. filtrationThe catalyst was filtered through a pad of celite
  2. washthe filter cake was washed with methanol
  3. customAfter the filtrate and washings were evaporated in vacuo
  4. customthe residue was recrystallized from methanol and diisopropyl ether
  5. customto give

출처 및 근거

ORD 기록
ord-38697a704d734ce28e1e5cc4764b35c7
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214824B2

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