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Trifluoroacetic acid → (5S)-5-Methyl-5-({[4-[(2-methylpyrimidin-5-yl)ethynyl]-3,6-dihydropyridin-1(2H)-yl]sulfonyl}methyl)imidazolidine-2,4-dione

HRID 1992328
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HRID 1992328 반응식
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([C:8]#[C:9][C:10]2[CH2:11][CH2:12][N:13](C(OC(C)(C)C)=O)[CH2:14][CH:15]=2)=[CH:4][N:3]=1.C(O)(C(F)(F)F)=O.C(N(C(C)C)C(C)C)C.[CH3:39][C@@:40]1([CH2:47][S:48](Cl)(=[O:50])=[O:49])[C:44](=[O:45])[NH:43][C:42](=[O:46])[NH:41]1>CCO.CN(C=O)C>[CH3:39][C@:40]1([CH2:47][S:48]([N:13]2[CH2:14][CH:15]=[C:10]([C:9]#[C:8][C:5]3[CH:6]=[N:7][C:2]([CH3:1])=[N:3][CH:4]=3)[CH2:11][CH2:12]2)(=[O:50])=[O:49])[NH:41][C:42](=[O:46])[NH:43][C:44]1=[O:45]
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참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 81531DiisopropylethylamineHCID 16738713(4S)-(4-methyl-2,5-dioxoimidazolidin-4-yl)methanesulphonyl chlorideHCID 86619012tert-Butyl 4-[(2-methylpyrimidin-5-yl)ethynyl]-3,6-dihydropyridine-1(2H)-carboxylate

생성물 1

HCID 11696764(5S)-5-Methyl-5-({[4-[(2-methylpyrimidin-5-yl)ethynyl]-3,6-dihydropyridin-1(2H)-yl]sulfonyl}methyl)imidazolidine-2,4-dione
수율 30%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6228Dimethylformamide용매

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온도
4 °C

실험 절차

tert-Butyl 4-[(2-methylpyrimidin-5-yl)ethynyl]-3,6-dihydropyridine-1(2H)-carboxylate was treated with TFA in EtOH and after completion of the reaction the solvent was evaporated and the mixture was freeze dried. The residue was taken up in DMF (1.5 mL) and the mixture was cooled to 4° C. N-Ethyldiisopropylamine (2.2 eq.) was added and the mixture was stirred for 20 minutes before adding [(4S)-4-methyl-2,5-dioxoimidazolidin-4-yl]methanesulfonyl chloride (Example 1f) (1.1 eq.) in DMF (1 mL). The mixture was stirred for 10 min at 4° C. and then stirred for 2 h at room temperature before the solvent was evaporated. The product was purified by preparative HPLC to give the title compound (0.022 g, 30%).

후처리

  1. customafter completion of the reaction the solvent
  2. customwas evaporated
  3. customdried
  4. stirringThe mixture was stirred for 10 min at 4° C.
  5. stirringstirred for 2 h at room temperature before the solvent
  6. customwas evaporated
  7. customThe product was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-b4bb68a655aa460f984ea7e12be051ef
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07648992B2

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