Ethanol → [1,1'-Biphenyl]-4-amine, 3-nitro-

HRID 859064

반응식

HRID 859064 반응식
[OH-].[K+].[N+:3]([C:6]1[CH:7]=[C:8]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:9]=[CH:10][C:11]=1[NH:12]C(=O)C)([O-:5])=[O:4].C(O)C>O>[N+:3]([C:6]1[CH:7]=[C:8]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:9]=[CH:10][C:11]=1[NH2:12])([O-:5])=[O:4]

참가 물질

5

반응물 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 79364Acetamide, N-(3-nitro(1,1'-biphenyl)-4-yl)-2회

생성물 1

HCID 77705[1,1'-Biphenyl]-4-amine, 3-nitro-수율 71.8%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A mixture of potassium hydroxide (2.5 g), 3-nitro-4-acetamido-1,1′-biphenyl (23.5 g), prepared in (A) above, water (6 mL) and ethanol (12 mL) is heated at reflux for one hour. The reaction mixture is cooled to room temperature and then poured into 300 mL of a mixture of water and ice. The solid is collected by filtration and the crude product is recrystallized from methanol (800 mL) to give 14.1 g of the title compound as an orange solid melting at 170–172° C.

후처리

  1. temperatureis heated
  2. temperatureat reflux for one hour
  3. filtrationThe solid is collected by filtration
  4. customthe crude product is recrystallized from methanol (800 mL)

출처 및 근거

ORD 기록
ord-4ca432c51406402ab157c2c7f9d916d4
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07148274B2

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