Hydrochloric Acid → 1-Hydroxy-6-nitro-2-indolinone

HRID 1007371

반응식

HRID 1007371 반응식
[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[CH2:13][C:14]([OH:16])=O)([O-])=[O:2].Cl.O.O.[Sn](Cl)Cl>C(O)C.O>[OH:2][N:1]1[C:4]2[C:5](=[CH:6][CH:7]=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=2)[CH2:13][C:14]1=[O:16]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 61436Stannous chloride dihydrate2회HCID 2215132,4-Dinitrophenylacetic acid

생성물 1

HCID 225695621-Hydroxy-6-nitro-2-indolinone

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

2.0 g of 2,4-dinitrophenylacetic acid (prepared according to J: Chem. Soc. 1948, 1717) are dissolved in 40 ml ethanol and 6.0 ml of conc. hydrochloric acid and 4.1 g of tin-(II)-chloride-dihydrate are added in batches at ambient temperature. The mixture is stirred for 12 hours at ambient temperature and for 4 hours at 60° C. After cooling another 2.0 g of tin-(II)-chloride-dihydrate are added and the mixture is stirred for another 12 hours at ambient temperature. The reaction mixture is diluted with water, extracted with methylene chloride and the organic phase is dried over sodium sulphate. After elimination of the solvent the residue is triturated with ether and the precipitate is filtered off.

후처리

  1. additionare added
  2. stirringthe mixture is stirred for another 12 hours at ambient temperature
  3. extractionextracted with methylene chloride
  4. dry with materialthe organic phase is dried over sodium sulphate
  5. customAfter elimination of the solvent the residue is triturated with ether
  6. filtrationthe precipitate is filtered off

출처 및 근거

ORD 기록
ord-8941d20d92524b6298ec0a406b10806a
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06794395B1

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