Hydrochloric Acid → Benzoic acid, 3,4-dihydroxy-5-nitro-, methyl ester

HRID 274439노트

반응식

HRID 274439 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]=1[OH:11])[C:5]([OH:7])=[O:6].Cl.[CH2:16](Cl)Cl>>[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]=1[OH:11])[C:5]([O:7][CH3:16])=[O:6]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 144509823,4-Dihydroxy-5-nitrobenzoic acid

생성물 1

HCID 5747973Benzoic acid, 3,4-dihydroxy-5-nitro-, methyl ester

실험 절차

1.0 g of 3,4-dihydroxy-5-nitrobenzoic acid is treated with 20 ml of methanolic hydrochloric acid, stirred at 45° for 3 hours and, after removing the solvent, the residue is taken up in methylene chloride. The organic phase is washed with sodium chloride solution, dried over sodium sulfate and evaporated. The crystalline product obtained is taken up in methylene chloride and filtered over a ten-fold amount of silica gel. The material obtained is recrystallized from ethyl acetate/n-hexane. There is obtained methyl 3,4-dihydroxy-5-nitrobenzoate in the form of yellow crystals of m.p. 144°-145°.

후처리

  1. customafter removing the solvent
  2. washThe organic phase is washed with sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. customThe crystalline product obtained
  6. filtrationfiltered over a ten-fold amount of silica gel
  7. customThe material obtained
  8. customis recrystallized from ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-baa77dbead454e65873427bc6fab6107
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389653

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