Hydrochloric Acid → HCID 22724458, 화합물

HRID 2086828노트

반응식

HRID 2086828 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([NH:13][C:14]1[CH:15]=[C:16]([NH:20][C:21]2[C:26]([N+:27]([O-])=O)=[CH:25][CH:24]=[CH:23][N:22]=2)[CH:17]=[CH:18][CH:19]=1)=[O:12].Cl.C(=O)(O)[O-].[Na+]>C(O)C.[Fe]>[NH2:27][C:26]1[C:21]([NH:20][C:16]2[CH:17]=[CH:18][CH:19]=[C:14]([NH:13][C:11]([C:2]3[CH:3]=[CH:4][C:5]4[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=4)[CH:1]=3)=[O:12])[CH:15]=2)=[N:22][CH:23]=[CH:24][CH:25]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 22724164HCID 22724164, 화합물

생성물 1

HCID 22724458HCID 22724458, 화합물수율 78%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

A mixture of 2-[3-(2-naphthoylamino)phenylamino]-3-nitropyridine (948 mg), iron powder (0.55 g) and hydrochloric acid (35%, 2 ml) in ethanol (8 ml) was stirred at 80° C. for 30 minutes. Then the mixture was poured into aqueous sodium bicarbonate and extracted with ethyl acetate twice. The combined organic phase was washed with aqueous sodium bicarbonate and brine, dried over magnesium sulfate and concentrated. The resultant solid was collected and washed with isopropyl ether to give 3-amino-2-[3-(2-naphthoylamino)phenylamino]pyridine (682 mg).

후처리

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

출처 및 근거

ORD 기록
ord-d034fe5fbd4349da87cc4a2c137a5a15
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06727245B2

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