Hydrochloric Acid → N2-(3-Chlorophenyl)-2,3-pyridinediamine

HRID 2086780노트

반응식

HRID 2086780 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[C:14]([N+:15]([O-])=O)=[CH:13][CH:12]=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1.Cl.C(=O)(O)[O-].[Na+]>C(O)C.[Fe]>[NH2:15][C:14]1[C:9]([NH:8][C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=2)=[N:10][CH:11]=[CH:12][CH:13]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 12588336HCID 12588336, 화합물

생성물 1

HCID 12588337N2-(3-Chlorophenyl)-2,3-pyridinediamine수율 81.1%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

A mixture of 2-(3-chlorophenylamino)-3-nitropyridine (394 mg), hydrochloric acid (35% 1.3 ml) and iron powder (0.44 g) in ethanol (5 ml) was refluxed for 15 minutes. The mixture was poured into aqueous sodium bicarbonate solution and extracted with ethyl acetate twice. The combined organic solution was washed with aqueous sodium bicarbonate solution and brine, dried over magnesium sulfate and concentrated. The resultant solid was collected and washed with isopropyl ether to give 3-amino-2-(3-chlorophenylamino)pyridine (281 mg).

후처리

  1. temperaturewas refluxed for 15 minutes
  2. extractionextracted with ethyl acetate twice
  3. washThe combined organic solution was washed with aqueous sodium bicarbonate solution and brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe resultant solid was collected
  7. washwashed with isopropyl ether

출처 및 근거

ORD 기록
ord-62545148ded04e09845814c12e7889e2
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06727245B2

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