2-Chlorobenzoyl chloride → 2-Chloro-benzoic acid N'-(5-fluoro-pyridin-2-yl)-hydrazide

HRID 75616

反応式

HRID 75616 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][NH2:9])=[N:6][CH:7]=1.[Cl:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13](Cl)=[O:14].CCN(C(C)C)C(C)C>C(Cl)Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][NH:9][C:13](=[O:14])[C:12]2[CH:16]=[CH:17][CH:18]=[CH:19][C:11]=2[Cl:10])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 691102-Chlorobenzoyl chlorideHCID 81531DiisopropylethylamineHCID 199167865-Fluoro-2-hydrazinylpyridine

生成物 1

HCID 866867222-Chloro-benzoic acid N'-(5-fluoro-pyridin-2-yl)-hydrazide収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of (5-fluoro-pyridin-2-yl)-hydrazine (for reference procedure see WO 2010/022076, which is incorporated herein by reference; 1.0 g, 7.87 mmol) and 2-chloro-benzoyl chloride (1 mL, 7.87 mmol) in DCM (50 mL) was added dropwise DIPEA (2.74 mL, 15.75 mmol). The reaction mixture was stirred at RT for 1 h then washed with water. The organic layer was dried through a phase separator and then concentrated in vacuo to afford the title compound (1.95 g, 93%) as a brown solid. LCMS (Method 3): Rt 2.82 min, m/z 266 [MH+].

後処理

  1. washthen washed with water
  2. customThe organic layer was dried through a phase separator
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b1fa1cc4ea254d9abf5af72b3c28aaca
出典データセット
uspto-grants-2014_09
特許番号
US08835431B2

関連ノート

読み込み中…