Nitric Acid → 2,4-Diamino-5-(3-amino-4-chloro-5-nitrophenyl)-6-ethylpyrimidine

HRID 53293

반응식

HRID 53293 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[C:4]([CH2:16][CH3:17])[N:3]=1.[N+:18]([O-])([OH:20])=[O:19].S(=O)(=O)(O)O>N>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[CH:10]=[CH:11][C:12]([Cl:15])=[C:13]([N+:18]([O-:20])=[O:19])[CH:14]=2)=[C:4]([CH2:16][CH3:17])[N:3]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 4993Pyrimethamine

생성물 1

HCID 3274042,4-Diamino-5-(3-amino-4-chloro-5-nitrophenyl)-6-ethylpyrimidine수율 93.8%

시약·촉매·용매 1

HCID 222Ammonia용매

반응 조건

온도
50 °C

실험 절차

2,4,-Diamino-5-(4-chlorophenyl)-6-ethylpyrimidine (103.8 g, 0.417 mol) ("Pyrimethamine" obtained from Sigma Chemical Co. Ltd.) was added in portions to a stirred mixture of concentrated nitric acid (210 ml) and concentrated sulphuric acid (210 ml). The mixture was heated at 50° C. for 1 h and then set aside at room temperature for 2.5 days. The reaction mixture was poured onto concentrated ammonia ("0.88" 5 dm3)/ice to effect a neutralisation. The resulting precipitate was collected by filtration and washed with water and sucked to dryness to give nitropyrimethamine as a yellow solid (115 g, 93.8% yield).

후처리

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed with water

출처 및 근거

ORD 기록
ord-440442055f414044a48cfebd69c9f0ec
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05618928

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