Methanesulfonyl chloride → Methanesulfonic acid 3-fluoro-pyridin-4-ylmethyl ester

HRID 426264ノート

反応式

HRID 426264 の反応式
[F:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH2:8][OH:9].[CH3:10][S:11](Cl)(=[O:13])=[O:12]>C(Cl)Cl>[F:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH2:8][O:9][S:11]([CH3:10])(=[O:13])=[O:12]

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 49760376(3-Fluoropyridin-4-yl)methanol

生成物 1

HCID 59184682Methanesulfonic acid 3-fluoro-pyridin-4-ylmethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

At 0° C. TEA (44 μl, 0.314 mmol, 2 eq.) was added to (3-fluoro-pyridin-4-yl)-methanol (20 mg, 0.157 mmol, 1 eq.) in 1 mL DCM, followed by MsCl (15 μl, 0.188 mmol, 1.2 eq.) The reaction was stirred at 0° C. for 30 minutes. HPLC and LC-MS showed reaction complete. The reaction crude was concentrated down. Ethyl acetate was added and washed with saturated NAHCO3 aqueous solution. The Ethyl acetate layer was concentrated after dried over Na2SO4 to give color oil which was used directly in next step. LC-MS shows 206.1 (M+1).

後処理

  1. customAt 0° C
  2. customreaction complete
  3. customThe reaction crude
  4. concentrationwas concentrated down
  5. additionEthyl acetate was added
  6. washwashed with saturated NAHCO3 aqueous solution
  7. concentrationThe Ethyl acetate layer was concentrated
  8. dry with materialafter dried over Na2SO4
  9. customto give color oil which

出典と根拠

ORDレコード
ord-a2a76b2d4c90488491a4697cea22b872
出典データセット
uspto-grants-2012_01
特許番号
US08106064B2

反応ノート

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