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

HRID 1007391ノート

反応式

HRID 1007391 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 added and the mixture is stirred for a total of 4 days at 50° C., adding, after 12 hours, a further 25.9 g of 1-chloro-2-dimethylamino-ethane, 49.8 g of potassium carbonate and 5.0 g of sodium iodide in 500 ml of acetone and, after 36 hours, a further 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. After this time the mixture is filtered and the filtrate is evaporated down. The residue is stirred with ether, suction filtered and dried at 40° C.

後処理

  1. additionadding, after 12 hours
  2. filtrationAfter this time the mixture is filtered
  3. customthe filtrate is 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-3646e7470ab44a5bad9b639145f0a7ae
出典データセット
uspto-grants-2004_09
特許番号
US06794395B1

反応ノート

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