Diisopropylethylamine → HCID 86649284, 화합물

HRID 450390

반응식

HRID 450390 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([N+:9]([O-:11])=[O:10])=[C:4](Cl)[N:3]=1.[CH3:13][C:14]1[NH:18][N:17]=[C:16]([NH2:19])[CH:15]=1.CC[N:22](C(C)C)C(C)C.N[C:30]1[CH:35]=[CH:34][O:33][CH2:32][CH:31]=1>CCO.O.CCOC(C)=O>[Cl:1][C:2]1[N:7]=[C:6]([N:19]([C:16]2[CH:15]=[C:14]([CH3:13])[NH:18][N:17]=2)[CH:30]2[CH2:35][CH2:34][O:33][CH2:32][CH2:31]2)[C:5]([N+:9]([O-:11])=[O:10])=[C:4]([NH2:22])[N:3]=1

참가 물질

8

반응물 4

HCID 81531DiisopropylethylamineHCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 42978432,4,6-Trichloro-5-nitropyrimidine2회HCID 17791271HCID 17791271, 화합물

생성물 1

HCID 86649284HCID 86649284, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2,4,6-trichloro-5-nitro pyrimidine (Intermediate 37, 1 g, 4.4 mmol) in EtOH at −50° C. were added 5-methyl-1H-pyrazol-3-amine (255 mg) and DIPEA (1.6 ml) drop-wise. The resulting mixture was stirred at this temperature for 5 minutes whereupon 4-amino pyran (300 mg) was added. The resulting mixture was allowed to warm to ambient temperature for 4 hours. The mixture was diluted with H2O and EtOAc and the aqueous layer was extracted with EtOAc. The combined organic layers were washed with brine, saturated NaHCO3 (aq) solution, dried and evaporation of the volatiles under reduced pressure gave a colored residue. Purification by Gilson (MeCN/H2O, 5%→95%, 15 minutes) gave the title compound (120 mg). LCMS: 354 [M+1].

후처리

  1. additionwas added
  2. extractionthe aqueous layer was extracted with EtOAc
  3. washThe combined organic layers were washed with brine, saturated NaHCO3 (aq) solution
  4. customdried
  5. customevaporation of the volatiles under reduced pressure
  6. customgave a colored residue
  7. customPurification by Gilson (MeCN/H2O, 5%→95%, 15 minutes)

출처 및 근거

ORD 기록
ord-0cac8eba3950473ca5dbaaedd86949aa
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486966B2

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