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

HRID 1350851ノート

反応式

HRID 1350851 の反応式
[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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-38697a704d734ce28e1e5cc4764b35c7
出典データセット
uspto-grants-2007_05
特許番号
US07214824B2

反応ノート

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