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

HRID 2185926노트

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HRID 2185926 반응식
[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]

참가 물질

3

반응물 1

HCID 28002414-Methoxy-3-nitrobenzonitrile

생성물 1

HCID 224525573-Amino-4-methoxybenzonitrile수율 94.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-57f4897fb02e4485a64ebc3cb255da9c
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06403594B1

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