Hydrochloric Acid → Diethyl 5-nitro-2-[2'-hydroxy-6'-sulphonaphthylazo]-phenylphosphonate

HRID 1277855

반응식

HRID 1277855 반응식
Br[C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[N:11]=[N:12][C:13]1[C:22]2[C:17](=[CH:18][C:19]([S:23]([O-:26])(=[O:25])=[O:24])=[CH:20][CH:21]=2)[CH:16]=[CH:15][C:14]=1[OH:27].[Na+].[CH2:29]([O:31][P:32]([OH:36])[O:33][CH2:34][CH3:35])[CH3:30].Cl>O>[N+:8]([C:6]1[CH:5]=[CH:4][C:3]([N:11]=[N:12][C:13]2[C:22]3[C:17](=[CH:18][C:19]([S:23]([OH:26])(=[O:25])=[O:24])=[CH:20][CH:21]=3)[CH:16]=[CH:15][C:14]=2[OH:27])=[C:2]([P:32](=[O:36])([O:33][CH2:34][CH3:35])[O:31][CH2:29][CH3:30])[CH:7]=1)([O-:10])=[O:9]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 12977Ethyl phosphite, (C2H5O)2(OH)PHCID 136359179Sodium 1-(2'-bromo-4'-nitrophenylazo)-2-hydroxy-6-naphthylsulphonate

생성물 1

HCID 136034815Diethyl 5-nitro-2-[2'-hydroxy-6'-sulphonaphthylazo]-phenylphosphonate

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

27 parts of sodium 1-(2'-bromo-4'-nitrophenylazo)-2-hydroxy-6-naphthylsulphonate are stirred with 130 ml of water, and 20 parts of copper sulphate 5-hydrate in 70 parts of water are added. The pH value is adjusted to 7-8 and the mixture is stirred for one hour. Thereafter, 35 parts of phosphorous acid diethyl ester are added dropwise at pH 8. The mixture is subsequently stirred at room temperature for 4 hours and acidified with hydrochloric acid. The precipitate is filtered off, washed and dried and gives 23 parts of diethyl 5-nitro-2-[2'-hydroxy-6'-sulphonaphthylazo]-phenylphosphonate almost free from starting compounds and by-products.

후처리

  1. additionare added
  2. stirringThe mixture is subsequently stirred at room temperature for 4 hours
  3. filtrationThe precipitate is filtered off
  4. washwashed
  5. customdried

출처 및 근거

ORD 기록
ord-adcdd8f9c6694af197811407fae52c96
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04279813

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