Hydrochloric Acid → HCID 19920903, 화합물

HRID 1647660노트

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HRID 1647660 반응식
N([O-])=O.[Na+].[CH3:5][S:6]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1N)(=[O:8])=[O:7].[ClH:17].[S:18](=[O:20])=[O:19]>O.[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.ClCCCl>[CH3:5][S:6]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[S:18]([Cl:17])(=[O:20])=[O:19])(=[O:8])=[O:7]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 1119Sulfur DioxideHCID 199209062-Aminophenyl methanesulfonateHCID 23668193Sodium Nitrite

생성물 1

HCID 19920903HCID 19920903, 화합물

시약·촉매·용매 3

HCID 66133Benzyl triethylammonium chloride촉매HCID 111,2-Dichloroethane용매HCID 962Water용매2회

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온도
0 °C

실험 절차

A diazonium salt solution, prepared by simultaneously introducing a solution of 39.5 g (0.57 mol) of sodium nitrite in 60 ml of water and 105 g (0.57 mol) of 2-aminophenyl methanesulfonate into 200 ml of concentrated hydrochloric acid at 0°-5° C. and stirring for 1 hour at 0° C., was added dropwise at 0°-10° C. to a solution, saturated with sulfur dioxide, of 1.7 g of CuCl2 and 4.5 g of benzyltriethylammonium chloride in 200 ml of 1,2-dichloroethane and 10 ml of water. The means of cooling were removed and stirring was carried out for 30 minutes at 25° C. and then, while slowly increasing the temperature of the reaction mixture, for a further hour at 50° C. The organic phase was separated off, washed with ice water and dried over Na2SO4. After removal of the solvent, an oily residue remained and could be crystallized by trituration with a little methanol. This gave 139 g (90% of theory) of the title compound of melting point 94°-95° C.

후처리

  1. temperatureof cooling
  2. customwere removed
  3. stirringstirring
  4. waitwas carried out for 30 minutes at 25° C.
  5. temperaturewhile slowly increasing the temperature of the reaction mixture
  6. waitfor a further hour at 50° C
  7. customThe organic phase was separated off
  8. washwashed with ice water
  9. dry with materialdried over Na2SO4
  10. customAfter removal of the solvent
  11. customcould be crystallized by trituration with a little methanol

출처 및 근거

ORD 기록
ord-3bb568d93207437e87f5362db4a1ad2d
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05434124

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