Hydrochloric Acid → 5-(3-Chlorosulfonylbenzenesulfonamido)-1-naphthol

HRID 1389902

반응식

HRID 1389902 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[C:7]2[OH:12].[C:13]1([S:23](Cl)(=[O:25])=[O:24])[CH:18]=[CH:17][CH:16]=[C:15]([S:19]([Cl:22])(=[O:21])=[O:20])[CH:14]=1.C(=O)([O-])O.[Na+].Cl>CO.C(#N)C>[Cl:22][S:19]([C:15]1[CH:14]=[C:13]([S:23]([NH:1][C:2]2[CH:11]=[CH:10][CH:9]=[C:8]3[C:3]=2[CH:4]=[CH:5][CH:6]=[C:7]3[OH:12])(=[O:25])=[O:24])[CH:18]=[CH:17][CH:16]=1)(=[O:20])=[O:21]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 657465-Amino-1-naphtholHCID 962401,3-Benzenedisulfonyl dichlorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 234607905-(3-Chlorosulfonylbenzenesulfonamido)-1-naphthol수율 55.3%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6342Acetonitrile용매

실험 절차

To a stirred mixture of 2.1 g of 5-amino-1-naphthol (1/2 H2SO4 salt), 4.2 g of benzene-1,3-disulfonyl chloride, 10 ml of acetonitrile and 30 ml of methanol was added portionwise 3.4 g of sodium hydrogen carbonate at a temperature of 0° to 5° C. The mixture was stirred for 1 hour at 0° to 5° C. and poured into 300 ml of a 3% hydrochloric acid aqueous solution. The precipitated crude product was collected by filtration and recrystallized from benzene-ethyl acetate (1:1 by volume) to produce 2.9 g of the title compound.

후처리

  1. customThe precipitated crude product
  2. filtrationwas collected by filtration
  3. customrecrystallized from benzene-ethyl acetate (1:1 by volume)

출처 및 근거

ORD 기록
ord-a1b4c7b81d2f4fc5b03f33142c92aaa6
출처 데이터셋
uspto-grants-1981_01
특허 번호
US04246414

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