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

HRID 1883724노트

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HRID 1883724 반응식
[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

참가 물질

6

반응물 4

HCID 5238Sodium Iodide3회HCID 79012-Chloro-N,N-dimethylethylamine3회HCID 11430Potassium Carbonate3회HCID 4689022N-(4-nitrophenyl)methanesulfonamide

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매3회

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온도
50 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-e1bed3ef037b4299b11ac0b4b457c9df
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06762180B1

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