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Diisopropylethylamine → HCID 71730367, 화합물

HRID 1056205
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HRID 1056205 반응식
C([NH:5]C1C(C)=NC2C(N=1)=C(C1NC3CN[C:23](=[O:24])C=3C=1)C=CC=2)(C)(C)C.Cl.[NH2:27][CH2:28][C:29]1[NH:30][C:31]([C:37]2[CH:46]=[CH:45][CH:44]=[C:43]3[C:38]=2[N:39]=[C:40]([NH:48][C:49]([CH3:52])([CH3:51])[CH3:50])[C:41]([CH3:47])=[N:42]3)=[CH:32][C:33]=1[C:34]([OH:36])=O.CCN(C(C)C)C(C)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N2CCCC2)(N2CCCC2)N2CCCC2)C2C=CC=CC=2N=N1>C(Cl)Cl.CN(C=O)C>[NH3:5].[CH3:23][OH:24].[C:49]([NH:48][C:40]1[C:41]([CH3:47])=[N:42][C:43]2[C:38]([N:39]=1)=[C:37]([C:31]1[NH:30][C:29]3[CH2:28][NH:27][C:34](=[O:36])[C:33]=3[CH:32]=1)[CH:46]=[CH:45][CH:44]=2)([CH3:52])([CH3:51])[CH3:50]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 71730367HCID 71730367, 화합물HCID 89783476HCID 89783476, 화합물

생성물 2

HCID 21705897Ammonia methanol수율 0%HCID 71730367HCID 71730367, 화합물수율 52%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매2회

실험 절차

Preparation 2-(3-(tert-butylamino)-2-methylquinoxalin-5-yl)-5,6-dihydropyrrolo[3,4-b]pyrrol-4(1H)-one (334). To a 100-mL round-bottomed flask was added 2-(aminomethyl)-5-(3-(tert-butylamino)-2-methylquinoxalin-5-yl)-1H-pyrrole-3-carboxylic acid hydrochloride (334c) (0.21 g, 0.55 mmol), DCM (10 mL), DMF (10 mL), DIEA (0.29 mL, 1.65 mmol), and (benzotriazol-1-yloxy)tripyrrolidinophosphonium hexafluorophosphate (0.34 g, 0.66 mmol) (Sigma-Aldrich Chemical Company, Inc.). The reaction mixture was stirred at RT for 30 min, concentrated to half of its volume, and diluted with EtOAc (10 mL). The organic extract was washed with sat NaHCO3 (5 mL), dried over Na2SO4, and concentrated. The crude material was absorbed onto a plug of silica gel and purified by chromatography through a Redi-Sep pre-packed silica gel column (12 g), eluted first with 30% EtOAc in hexanes, and then with a gradient of 0-4% 2 M NH3/MeOH in DCM to provide 2-(3-(tert-butylamino)-2-methylquinoxalin-5-yl)-5,6-dihydropyrrolo[3,4-b]pyrrol-4(1H)-one (334) (97 mg, 52% yield) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ 12.08 (br. s., 1H), 7.82 (d, J=7.24 Hz, 1H), 7.63 (d, J=8.02 Hz, 1H), 7.53 (s, 1H), 7.37 (t, J=7.73 Hz, 1H), 6.94 (s, 1H), 6.02 (s, 1H), 4.29 (s, 2H), 2.58 (s, 3H), 1.55 (s, 9H). m/z (ESI, +ve) 336.2 (M+H)+.

후처리

  1. concentrationconcentrated to half of its volume
  2. additiondiluted with EtOAc (10 mL)
  3. extractionThe organic extract
  4. washwas washed with sat NaHCO3 (5 mL)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customThe crude material was absorbed onto a plug of silica gel
  8. custompurified by chromatography through a Redi-Sep pre-packed silica gel column (12 g)
  9. washeluted first with 30% EtOAc in hexanes

출처 및 근거

ORD 기록
ord-db01a97807e9474896c5d9db4f1306b9
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394297B2

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