Methanesulfonyl chloride → 3-Bromo-5-(1-(methylsulfonyl)pyrrolidin-3-yl)pyridin-2-amine

HRID 595820ノート

反応式

HRID 595820 の反応式
[Br:1][C:2]1[C:3]([NH2:13])=[N:4][CH:5]=[C:6]([CH:8]2[CH2:12][CH2:11][NH:10][CH2:9]2)[CH:7]=1.CCN(C(C)C)C(C)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25]>C(Cl)Cl>[Br:1][C:2]1[C:3]([NH2:13])=[N:4][CH:5]=[C:6]([CH:8]2[CH2:12][CH2:11][N:10]([S:24]([CH3:23])(=[O:26])=[O:25])[CH2:9]2)[CH:7]=1

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 1180452883-Bromo-5-(pyrrolidin-3-yl)pyridin-2-amine

生成物 1

HCID 1180455673-Bromo-5-(1-(methylsulfonyl)pyrrolidin-3-yl)pyridin-2-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 3-bromo-5-(pyrrolidin-3-yl)pyridin-2-amine (20 mg, 0.083 mmol) in DCM in ice bath was added DIEA (57.7 μl, 0.330 mmol) and methanesulfonyl chloride (7.08 μl, 0.091 mmol). The reaction mixture was stirred in ice bath 30 min. The reaction mixture was partitioned between DCM and water. The DCM layer was separated and washed with brine, dried over sodium sulfate, filtered and evaporated. The crude product was used for next step without purification. LCMS (m/z): 320.0/322.0 (MH+), 0.363 min.

後処理

  1. customThe reaction mixture was partitioned between DCM and water
  2. customThe DCM layer was separated
  3. washwashed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude product was used for next step without purification
  8. custom320.0/322.0 (MH+), 0.363 min.

出典と根拠

ORDレコード
ord-d28dfc69b41442eab8c81176aa824a16
出典データセット
uspto-grants-2016_01
特許番号
US09242996B2

反応ノート

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