Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → 2-(6-Fluoro-4-iodopyridin-3-ylamino)ethanol

HRID 1640909ノート

反応式

HRID 1640909 の反応式
[F:1][C:2]1[N:7]=[CH:6][C:5]([NH:8][CH2:9][CH2:10][O:11]C2CCCCO2)=[C:4]([I:18])[CH:3]=1.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>C(O)C>[F:1][C:2]1[N:7]=[CH:6][C:5]([NH:8][CH2:9][CH2:10][OH:11])=[C:4]([I:18])[CH:3]=1

参加物

4

反応物 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 667381816-Fluoro-4-iodo-N-(2-(tetrahydro-2H-pyran-2-yloxy)ethyl)pyridin-3-amine

生成物 1

HCID 667381242-(6-Fluoro-4-iodopyridin-3-ylamino)ethanol収率 28.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

Dissolve 6-fluoro-4-iodo-N-(2-(tetrahydro-2H-pyran-2-yloxy)ethyl)pyridin-3-amine (0.20 g, 0.55 mmol) in ethanol (5.5 mL). Add pyridinium p-toluenesulfonate (0.014 g, 0.055 mmol). Heat the reaction mixture at 50° C. overnight. Remove the solvent under reduced pressure. Purify by FCC (0.1% to 1% 2 M NH3 methanol solution/CH2Cl2) to give the title compound (44 mg, 28%) with 100% HPLC purity. MS (ES) m/z 283 [M+1]+.

後処理

  1. customRemove the solvent under reduced pressure
  2. customPurify by FCC (0.1% to 1% 2 M NH3 methanol solution/CH2Cl2)

出典と根拠

ORDレコード
ord-5419aa4a55b24bb9bebf547acc753e23
出典データセット
uspto-grants-2012_02
特許番号
US08114872B2

反応ノート

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