4-Methoxy-3-nitrobenzonitrile → 3-Amino-4-methoxybenzonitrile

HRID 2185926ノート

反応式

HRID 2185926 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:12][CH3:13])=[C:7]([N+:9]([O-])=O)[CH:8]=1)#[N:2]>C(O)C>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:12][CH3:13])=[C:7]([CH:8]=1)[NH2:9])#[N:2]

参加物

3

反応物 1

HCID 28002414-Methoxy-3-nitrobenzonitrile

生成物 1

HCID 224525573-Amino-4-methoxybenzonitrile収率 94.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 8.8 g of Compound 18A and 46.8 g of stannous chloride dihydrate in 250 mL of 95% ethanol was refluxed for 1 hour. The solvent was evaporated off in vacuo and the residue was taken up with 200 mL of water. The mixture was acidified with 37% HCl, then alkalinised with 35% sodium hydroxide and extracted with 3×200 mL of diethyl ether. The combined organic layers were washed with 50 mL of water, dried over sodium sulphate and evaporated to dryness in vacuo to afford 6.90 g (94.2%) of Compound 18B as an ivory solid.

後処理

  1. temperaturewas refluxed for 1 hour
  2. customThe solvent was evaporated off in vacuo
  3. extractionextracted with 3×200 mL of diethyl ether
  4. washThe combined organic layers were washed with 50 mL of water
  5. dry with materialdried over sodium sulphate
  6. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-57f4897fb02e4485a64ebc3cb255da9c
出典データセット
uspto-grants-2002_06
特許番号
US06403594B1

反応ノート

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