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

HRID 1007371

反応式

HRID 1007371 の反応式
[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]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 61436Stannous chloride dihydrate2 回HCID 2215132,4-Dinitrophenylacetic acid

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8941d20d92524b6298ec0a406b10806a
出典データセット
uspto-grants-2004_09
特許番号
US06794395B1

関連ノート

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