Hydrochloric Acid → 6-Nitropyrido[2,3-d]pyrimidine-2,4-diamine

HRID 1417200

반응식

HRID 1417200 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([NH2:9])[N:3]=1.Cl.[N+:11]([CH:14]([CH:17]=O)[CH:15]=O)([O-:13])=[O:12]>C(O)C>[NH2:1][C:2]1[N:3]=[C:4]([NH2:9])[C:5]2[CH:17]=[C:14]([N+:11]([O-:13])=[O:12])[CH:15]=[N:8][C:6]=2[N:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 138632,4,6-TriaminopyrimidineHCID 313475Nitromalonaldehyde

생성물 1

HCID 110527766-Nitropyrido[2,3-d]pyrimidine-2,4-diamine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

About 1 equivalent of 2,4,6-triamino pyrimidine was suspended in about 50 ml of refluxing absolute ethanol with stirring under an atmosphere of nitrogen. Concentrated HCl was added dropwise to effect solution and as soon as solution occurred, about 1.2 equivalents of nitromalonaldehyde was added all at once. Within 10 minutes, a thick reddish voluminous precipitate started forming. TLC analysis indicated the presence of a yellow spot corresponding to that of the desired product along with staring materials. The reaction mixture was stirred at reflux for 3.5 hours, immediately diluted with 30 ml of water, cooled and neutralized with concentrated NH4OH. The precipitate was collected on a funnel and was washed repeatedly with water to remove unreacted triamino pyrimidine to yield pure 2,4-diamino-6-nitropyrido[2,3-d]pyrimidine.

후처리

  1. customa thick reddish voluminous precipitate started forming

출처 및 근거

ORD 기록
ord-982f3efc8b7146268e8990b1a23a0297
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05877178

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