Hydrochloric Acid → HCID 67046796、化合物

HRID 1438388ノート

反応式

HRID 1438388 の反応式
[CH3:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].N1C=C[CH:12]=[CH:11][CH:10]=1.[CH3:15][S:16](Cl)(=[O:18])=[O:17].[Cl-].[Cl-].[Cl-].[Al+3].C(Cl)(=[O:26])C.Cl>C(Cl)Cl.C1(C)C=CC=CC=1.O>[CH3:1][C:2]1[CH:8]=[C:7]([C:10](=[O:26])[CH2:11][CH3:12])[CH:6]=[CH:5][C:3]=1[NH:4][S:16]([CH3:15])(=[O:18])=[O:17]

参加物

10

反応物 6

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6367Acetyl chlorideHCID 7242O-ToluidineHCID 31297Methanesulfonyl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 67046796HCID 67046796、化合物収率 43.5%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-methylaniline (2.2 g, 20 mmol, purchased from TCl) in pyridine (1.7 ml. 1.7 g, 21.4 mmol) and DCM (85 ml), methanesulfonyl chloride (1.6 ml, 2.3 g, 20 mmol) was added dropwise over 10 minutes at 0° C. The reaction mixture was stirred at room temperature for 1 hour. After cooling to 0° C., aluminum trichloride (6.8 g, 51 mmol) was added to the reaction mixture carefully. Then acetyl chloride (1.9 g, 20 mmol) was added dropwise over 15 minutes. The reaction mixture was diluted with toluene (25 ml) and poured into 2 M HCl aqueous solution (500 ml) with stirring at 0° C. The precipitates were filtered,washed with water and dried in vacuo to afford the title compound (2.1 g, 43%) as yellow solids.

後処理

  1. temperatureAfter cooling to 0° C.
  2. stirringwith stirring at 0° C
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-a2aa513e62a8444a9972517ce52a7586
出典データセット
uspto-grants-2009_11
特許番号
US07622589B2

反応ノート

読み込み中…