1,2-Dichloroethane → N'-(6-chloropyridazin-3-yl)-2-(7-methoxyquinolin-4-yloxy)acetohydrazide

HRID 40175

反応式

HRID 40175 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1.ON1C2N=CC=CC=2N=N1.C(Cl)CCl.[CH3:24][O:25][C:26]1[CH:35]=[C:34]2[C:29]([C:30]([O:36][CH2:37][C:38](O)=[O:39])=[CH:31][CH:32]=[N:33]2)=[CH:28][CH:27]=1.C(N(C(C)C)CC)(C)C>CN(C=O)C>[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][NH:9][C:38](=[O:39])[CH2:37][O:36][C:30]2[C:29]3[C:34](=[CH:35][C:26]([O:25][CH3:24])=[CH:27][CH:28]=3)[N:33]=[CH:32][CH:31]=2)=[CH:4][CH:3]=1

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 81531DiisopropylethylamineHCID 1007873-Chloro-6-hydrazinopyridazineHCID 181649HOAtHCID 576910212-(7-Methoxyquinolin-4-yloxy)acetic acid

生成物 1

HCID 86630262N'-(6-chloropyridazin-3-yl)-2-(7-methoxyquinolin-4-yloxy)acetohydrazide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

A mixture of 1-(6-chloropyridazin-3-yl)hydrazine (0.372 g, 2.57 mmol), 1-hydroxy-7-aza-benzotriazole (0.350 g, 2.57 mmol), EDC (0.641 g, 3.34 mmol), 2-(7-methoxyquinolin-4-yloxy)acetic acid (0.600 g, 2.57 mmol) and diisopropylethylamine (1.34 ml, 7.72 mmol) in DMF (20 mL) was allowed to stir at 50° C. for 2 h. Concentrated. Reconstitued in MeCN (30 mL). Concentrated with cooling. Product crashed out of solution and was isolated by filtration. Used without further purification. (ESI, pos. ion) m/z: 234.1 (M+H).

後処理

  1. concentrationConcentrated
  2. concentrationConcentrated
  3. temperaturewith cooling
  4. customwas isolated by filtration
  5. customUsed without further purification

出典と根拠

ORDレコード
ord-fc76c502eb6d407db4f6272427ad0b0f
出典データセット
uspto-grants-2013_09
特許番号
US08524900B2

関連ノート

読み込み中…