Ammonia → 3-[(2-Dimethylamino-4-nitro-benzoyl)-amino]-2-amino-6-methoxy-pyridine

HRID 3851ノート

反応式

HRID 3851 の反応式
[CH3:1][N:2]([CH3:15])[C:3]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=O.Cl.Cl.[NH2:18][C:19]1[C:24]([NH2:25])=[CH:23][CH:22]=[C:21]([O:26][CH3:27])[N:20]=1.O.N>P(Cl)(Cl)(Cl)=O>[CH3:15][N:2]([CH3:1])[C:3]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:4]=1[C:5]([NH:25][C:24]1[C:19]([NH2:18])=[N:20][C:21]([O:26][CH3:27])=[CH:22][CH:23]=1)=[O:7]

参加物

6

反応物 4

HCID 222AmmoniaHCID 962WaterHCID 30239192,3-Diamino-6-methoxypyridine dihydrochlorideHCID 201382202-(Dimethylamino)-4-nitrobenzoic acid

生成物 1

HCID 135324023-[(2-Dimethylamino-4-nitro-benzoyl)-amino]-2-amino-6-methoxy-pyridine

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

An amount of 1.05 gm of 2-dimethylamino-4-nitro-benzoic acid is suspended in 35 ml of phosphorus oxychloride, and 1.05 gm of 2,3-diamino-6-methoxy-pyridine dihydrochloride are added thereto. The mixture is refluxed for 5 minutes, left to cool for 15 minutes with stirring, and finally decomposed with water. The solution obtained is cooled and poured onto a mixture of ice and concentrated ammonia. The product is then precipitated. It is subjected to suction filtration, washed with water, and dried in a circulating air drier at 50° C.

後処理

  1. temperatureThe mixture is refluxed for 5 minutes
  2. waitleft
  3. temperatureto cool for 15 minutes
  4. customThe solution obtained
  5. temperatureis cooled
  6. customThe product is then precipitated
  7. filtrationIt is subjected to suction filtration
  8. washwashed with water
  9. customdried in a circulating air drier at 50° C.

出典と根拠

ORDレコード
ord-ed32d25e0c7c45dfb2b09ee2c01e0cd2
出典データセット
uspto-grants-1988_02
特許番号
US04722929

反応ノート

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