Water → HCID 178494417、化合物
反応式
[CH3:1][O:2][C:3]1([OH:20])[CH:8]=[C:7]([O:9]C)[N:6]=[C:5]([C:11]2[S:12][CH:13]=[C:14]([C:16]([F:19])([F:18])[F:17])[N:15]=2)[NH:4]1.B(Cl)(Cl)Cl.O.C(Cl)Cl>ClCCCl>[OH:9][C:7]1[N:6]=[C:5]([C:11]2[S:12][CH:13]=[C:14]([C:16]([F:19])([F:18])[F:17])[N:15]=2)[NH:4][C:3]([O:2][CH3:1])([OH:20])[CH:8]=1参加物
6
反応条件
- 温度
- 60 °C
実験手順
To a solution of compound 288 (460 mg, 1 eq.) in DCE (10 mL) was added BCl3 (3.16 mL, 2 eq.). The mixture was stirred at 60° C. for 16 hrs. Water and DCM were then added. Organics were separated, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was triturated in a DCM/pentane mixture to yield compound 289 as a beige solid in 38% yield. MS (ESI, EI+): m/z=278 (MH+).
後処理
- customOrganics were separated
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was triturated in a DCM/pentane mixture
出典と根拠
- ORDレコード
- ord-295f7650f800461aa1ec0e835cae4b02
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09353100B2
反応ノート
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