Water → Thiazosulfone

HRID 1656937

반응식

HRID 1656937 반응식
[NH2:1][C:2]1[S:3][C:4]([S:7]([C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][CH:11]=2)(=[O:9])=[O:8])=[CH:5][N:6]=1.[Cl-].[NH4+].O1CCCC1.O>C(O)C.[Fe]>[NH2:1][C:2]1[S:3][C:4]([S:7]([C:10]2[CH:15]=[CH:14][C:13]([NH2:16])=[CH:12][CH:11]=2)(=[O:9])=[O:8])=[CH:5][N:6]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 1535p-Nitrophenyl-2-aminothiazol-5-ylsulphoneHCID 8028TetrahydrofuranHCID 25517Ammonium Chloride

생성물 1

HCID 10124Thiazosulfone수율 86.6%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

To a mixture of 2-amino-5-(4-nitrophenylsulfonyl)thiazole (4.0 g) and ammonium chloride in a mixture of ethanol (80 ml), tetrahydrofuran (40 ml) and water (30 ml) was portionwise added the iron powder (4 g) at 80° C. with stirring. The mixture was refluxed for 1.5 hours with stirring. The reaction mixture was filtered by suction and the filtrate was concentrated under reduced pressure. The residue was triturated with water and the precipitates were collected by filtration, washed with water and dried in vacuo to give 2-amino-5-(4-aminophenylsulfonyl)thiazole (3.10 g, yield: 86.6%). mp: 218°-219° C. IR (Nujol): 3400, 3300, 1620, 1595, 1535, 1380 cm-1

후처리

  1. temperatureThe mixture was refluxed for 1.5 hours
  2. stirringwith stirring
  3. filtrationThe reaction mixture was filtered by suction
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was triturated with water
  6. filtrationthe precipitates were collected by filtration
  7. washwashed with water
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-19f5e8ca25f6489b975e4ba86a3c07e1
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05256675

연결된 노트

불러오는 중…