Hydrochloric Acid → 4-Hydrazino-1-naphthalenesulphonic acid hydrochloride

HRID 1081442

반응식

HRID 1081442 반응식
[OH-].[Na+].[NH2:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([S:14]([OH:17])(=[O:16])=[O:15])=[CH:6][CH:5]=1.[N:18]([O-])=O.[Na+].[ClH:22]>O>[ClH:22].[NH:3]([C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([S:14]([OH:17])(=[O:15])=[O:16])=[CH:6][CH:5]=1)[NH2:18]

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 67904-Amino-1-naphthalenesulfonic acidHCID 14798Sodium Hydroxide2회HCID 23668193Sodium Nitrite

생성물 1

HCID 867493604-Hydrazino-1-naphthalenesulphonic acid hydrochloride

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

4 g of NaOH are added to a suspension of 22.33 g of 4-amino-1-naphthalenesulphonic acid in 125 ml of water. The mixture is cooled to 0° C. and 2 ml of concentrated NaOH are added, followed by 7.5 g of sodium nitrite and 125 g of ice to maintain the temperature at 0° C. The suspension thereby obtained is poured into 75 ml of concentrated HCl cooled beforehand to 0° C., and left stirring for 2 hours 15 minutes at this temperature. The reaction mixture is added slowly to a solution, cooled beforehand to -10° C., of 55 g of stannous chloride dihydrate in 50 ml of concentrated HCl and 25 ml of water. After one night, the expected product is obtained by filtration, rinsing with 1N HCl and with water, m=23.96 g.

후처리

  1. temperatureto maintain the temperature at 0° C
  2. customThe suspension thereby obtained
  3. temperaturecooled beforehand to 0° C.
  4. waitleft
  5. additionThe reaction mixture is added slowly to a solution
  6. waitAfter one night

출처 및 근거

ORD 기록
ord-5f3ef10ff16a4b12b8d4fc75aae20cc1
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05585497

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