Acetic Acid → 3-Amino-2-bromobenzonitrile

HRID 2275223노트

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HRID 2275223 반응식
[Br:1][C:2]1[C:9]([N+:10]([O-])=O)=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].C(O)(=O)C.[OH-].[Na+]>C(O)C.O.[Fe]>[NH2:10][C:9]1[C:2]([Br:1])=[C:3]([CH:6]=[CH:7][CH:8]=1)[C:4]#[N:5]

참가 물질

7

반응물 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 131624152-Bromo-3-nitrobenzonitrile

생성물 1

HCID 601554243-Amino-2-bromobenzonitrile

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

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온도
60 °C

실험 절차

2-Bromo-3-nitro-benzonitrile (Compound U1, 678 mg, 2.987 mmol) was dissolved in ethanol (20.9 mL) and water (8.96 mL), added with acetic acid (2.39 mL, 41.81 mmol) and iron (1.17 g, 20.91 mmol), and stirred at 60° C. for 18 hr. The reaction solution was poured into aqueous solution of sodium hydroxide (1 M), extracted with ethyl acetate, washed with water and saturated brine, dried over sodium sulfate, and then filtered. After concentration under reduced pressure, 3-amino-2-bromo-benzonitrile (Compound U2) was obtained as a crude product.

후처리

  1. extractionextracted with ethyl acetate
  2. washwashed with water and saturated brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationAfter concentration under reduced pressure

출처 및 근거

ORD 기록
ord-7cedb54ddbb94c31b7a8d9fddc8c34e2
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126931B2

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