Hydrochloric Acid → HCID 22724458、化合物

HRID 2231004ノート

反応式

HRID 2231004 の反応式
[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

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 22724164HCID 22724164、化合物

生成物 1

HCID 22724458HCID 22724458、化合物収率 78%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-cb6080cb1db54ac4960895b263d41c4b
出典データセット
uspto-grants-2002_07
特許番号
US06426345B1

反応ノート

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