Ammonium Chloride → HCID 84665992、化合物

HRID 2208918ノート

反応式

HRID 2208918 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N+:14]([O-])=O)[C:6]([CH3:13])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9].[Cl-].[NH4+]>C(O)C.O.[Fe]>[NH2:14][C:5]1[C:6]([CH3:13])=[C:7]([CH:12]=[C:3]([O:2][CH3:1])[CH:4]=1)[C:8]([O:10][CH3:11])=[O:9]

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 53399479Benzoic acid, 5-methoxy-2-methyl-3-nitro-, methyl ester

生成物 1

HCID 84665992HCID 84665992、化合物収率 80.9%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a stirred solution of methyl 5-methoxy-2-methyl-3-nitrobenzoate (1.7 g, 7.6 mmol) in ethanol (20 mL) was added ammonium chloride (1.7 g, 32 mmol) dissolved in water (20 mL) and iron powder (3.38 g, 60.44 mmol). The mixture was heated at 80° C. for 3 h, filtered and the residue washed well with hot ethanol. The filtrate was concentrated and the residue was basified with aqueous sodium bicarbonate. The aqueous phase was extracted with ethyl acetate. The combined organic layers were washed with water, dried, and concentrated under reduced pressure to give the crude title compound (1.2 g) which was used directly in the next step.

後処理

  1. filtrationfiltered
  2. washthe residue washed well with hot ethanol
  3. concentrationThe filtrate was concentrated
  4. extractionThe aqueous phase was extracted with ethyl acetate
  5. washThe combined organic layers were washed with water
  6. customdried
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-4eeb3cc9326e4c23b233baf73eaf3899
出典データセット
uspto-grants-2016_06
特許番号
US09376422B2

反応ノート

読み込み中…