Diisopropylethylamine → HCID 178454304, 화합물

HRID 1247785노트

반응식

HRID 1247785 반응식
S(=O)(=O)(O)O.[NH2:6][C:7]1[CH:8]=[N:9][N:10]2[CH2:15][CH2:14][CH2:13][NH:12][C:11]=12.C(N(C(C)C)C(C)C)C.[C:25]([O:29][C:30]([NH:32][C:33]([NH:42][C:43]([O:45][C:46]([CH3:49])([CH3:48])[CH3:47])=[O:44])=NS(C(F)(F)F)(=O)=O)=[O:31])([CH3:28])([CH3:27])[CH3:26]>C(Cl)Cl>[C:46]([O:45][C:43]([N:42]=[C:33]([NH:32][C:30]([O:29][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:31])[NH:6][C:7]1[CH:8]=[N:9][N:10]2[CH2:15][CH2:14][CH2:13][NH:12][C:11]=12)=[O:44])([CH3:49])([CH3:48])[CH3:47]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 36945701,3-Di-Boc-2-(trifluoromethylsulfonyl)guanidineHCID 1358007334,5,6,7-Tetrahydropyrazolo[1,5-a]pyrimidin-3-amine sulfate

생성물 1

HCID 178454304HCID 178454304, 화합물수율 89.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-amino-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine sulfuric acid salt (2.96 g) and N-ethyldiisopropylamine (3.88 g) in methylene chloride (70 ml) was added 1,3-bis(tert-butoxycarbonyl)-2-(trifluoromethanesulfonyl)guanidine (3.91 g). The mixture was stirred at room temperature for 150 minutes. There action mixture was washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with 2% methanol/chloroform to give 3-[2,3-bis(tert-butoxycarbonyl)guanidino]-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine (3.4 g) as a solid.

후처리

  1. washThere action mixture was washed with saturated aqueous sodium hydrogen carbonate solution
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel eluting with 2% methanol/chloroform

출처 및 근거

ORD 기록
ord-22f303c04b084084be1e7bb0a94314b1
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129232B2

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