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

HRID 3851노트

반응식

HRID 3851 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-ed32d25e0c7c45dfb2b09ee2c01e0cd2
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722929

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