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

HRID 274439ノート

反応式

HRID 274439 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-baa77dbead454e65873427bc6fab6107
出典データセット
uspto-grants-1995_02
特許番号
US05389653

反応ノート

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