Diisopropylethylamine → HCID 86649284、化合物

HRID 450390

反応式

HRID 450390 の反応式
[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

参加物

8

反応物 4

HCID 81531DiisopropylethylamineHCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 42978432,4,6-Trichloro-5-nitropyrimidine2 回HCID 17791271HCID 17791271、化合物

生成物 1

HCID 86649284HCID 86649284、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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].

後処理

  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)

出典と根拠

ORDレコード
ord-0cac8eba3950473ca5dbaaedd86949aa
出典データセット
uspto-grants-2013_07
特許番号
US08486966B2

関連ノート

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