Sodium Iodide → N-(2-dimethylamino-ethyl)-N-methylsulphonyl-4-nitroaniline

HRID 1883724ノート

反応式

HRID 1883724 の反応式
[CH3:1][S:2]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1)(=[O:4])=[O:3].Cl[CH2:16][CH2:17][N:18]([CH3:20])[CH3:19].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CC(C)=O>[CH3:19][N:18]([CH3:20])[CH2:17][CH2:16][N:5]([S:2]([CH3:1])(=[O:3])=[O:4])[C:6]1[CH:7]=[CH:8][C:9]([N+:12]([O-:14])=[O:13])=[CH:10][CH:11]=1

参加物

6

反応物 4

HCID 5238Sodium Iodide3 回HCID 79012-Chloro-N,N-dimethylethylamine3 回HCID 11430Potassium Carbonate3 回HCID 4689022N-(4-nitrophenyl)methanesulfonamide

生成物 1

HCID 22668565N-(2-dimethylamino-ethyl)-N-methylsulphonyl-4-nitroaniline

試薬・触媒・溶媒 1

HCID 180Acetone溶媒3 回

反応条件

温度
50 °C

実験手順

38.9 g of N-methylsulphonyl-4-nitroaniline are dissolved in 2.0 l of acetone, 51.9 g of 1-chloro-2-dimethylamino-ethane, 77.4 g of potassium carbonate and 5.0 g of sodium iodide are added and the mixture is stirred for a total of 4 days at 50° C., while after 12 hours a further 25.9 g of 1-chloro-2dimethylamino-ethane, 49.8 g of potassium carbonate and 5.0 g of sodium iodide in 500 ml of acetone are added and after 36 hours another 26.0 g of 1-chloro-2-dimethylamino-ethane, 50.0 g of potassium carbonate and 5.0 g of sodium iodide in 100 ml of acetone are added. After this time the mixture is filtered and the filtrate evaporated down. The residue is stirred with ether, suction filtered and dried at 40° C.

後処理

  1. additionare added
  2. filtrationAfter this time the mixture is filtered
  3. customthe filtrate evaporated down
  4. stirringThe residue is stirred with ether, suction
  5. filtrationfiltered
  6. customdried at 40° C.

出典と根拠

ORDレコード
ord-e1bed3ef037b4299b11ac0b4b457c9df
出典データセット
uspto-grants-2004_07
特許番号
US06762180B1

反応ノート

読み込み中…