Methanesulfonyl chloride → N-(3-(6-chloro-4-iodopyridin-2-ylamino)cyclohexyl)methanesulfonamide

HRID 390102

反応式

HRID 390102 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH:9]2[CH2:14][CH2:13][CH2:12][CH:11]([NH2:15])[CH2:10]2)[CH:5]=[C:4]([I:16])[CH:3]=1.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>N1C=CC=CC=1>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH:9]2[CH2:14][CH2:13][CH2:12][CH:11]([NH:15][S:18]([CH3:17])(=[O:20])=[O:19])[CH2:10]2)[CH:5]=[C:4]([I:16])[CH:3]=1

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 86649873N1-(6-chloro-4-iodopyridin-2-yl)cyclohexane-1,3-diamine

生成物 1

HCID 87178324N-(3-(6-chloro-4-iodopyridin-2-ylamino)cyclohexyl)methanesulfonamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of EXAMPLE 11A (100 mg, 0.3 mmol) in pyridine (5 mL) was added methanesulfonyl chloride (50 mg, 0.4 mmol). The mixture was stirred at ambient temperature for 5 h and partitioned between ethyl acetate and brine. The organic phase was washed with brine and concentrated. The residue was purified by flash chromatography on silica gel eluting with ethyl acetate to provide the title compound. Yield: 100 mg (82%). MS (DCI/NH3) m/z 430 (M+H)+.

後処理

  1. custompartitioned between ethyl acetate and brine
  2. washThe organic phase was washed with brine
  3. concentrationconcentrated
  4. customThe residue was purified by flash chromatography on silica gel eluting with ethyl acetate

出典と根拠

ORDレコード
ord-9a914a045aa04c59866671a9903bff04
出典データセット
uspto-grants-2013_02
特許番号
US08383624B2

関連ノート

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