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Diisopropylethylamine → HCID 25126143, 화합물

HRID 1875002
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HRID 1875002 반응식
[Br:1][C:2]1[CH:6]=[CH:5][NH:4][C:3]=1[C:7]([OH:9])=O.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[NH2:43][CH2:44][C:45]1[C:46]([F:62])=[C:47]([O:52][C:53]2[CH:54]=[C:55]([CH:58]=[C:59]([Cl:61])[CH:60]=2)[C:56]#[N:57])[C:48]([Cl:51])=[CH:49][CH:50]=1>CN(C=O)C.CCOC(C)=O.O>[Br:1][C:2]1[CH:6]=[CH:5][NH:4][C:3]=1[C:7]([NH:43][CH2:44][C:45]1[CH:50]=[CH:49][C:48]([Cl:51])=[C:47]([O:52][C:53]2[CH:54]=[C:55]([C:56]#[N:57])[CH:58]=[C:59]([Cl:61])[CH:60]=2)[C:46]=1[F:62])=[O:9]
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참가 물질

8

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 538307483-bromo-1H-pyrrole-2-carboxylic acidHCID 594513923-{[3-(Aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile

생성물 1

HCID 25126143HCID 25126143, 화합물수율 8.8%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3-bromo-1H-pyrrole-2-carboxylic acid (0.2 g, 0.684 mmol) in DMF (2 mL) was added HATU (0.48 g, 1.262 mmol), DIPEA (0.270 ml, 1.547 mmol) and 3-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile (0.39 g, 1.253 mmol). The reaction mixture was stirred at RT overnight. Water (5 ml) and EtOAc (10 mL) were added and the layers separated. The aqueous layer was extracted with EtOAc (3×10 mL), the organic layers combined, dried over sodium sulfate, filtered and evaporated. Purification was accomplished by RPHPLC. Further purification by RPHPLC was required. The desired fractions were collected, neutralized with sat. sodium bicarbonate and extracted with EtOAc (3×10 mL). The organic layers were combined, dried over sodium sulfate, filtered and evaporated to afford 3-bromo-N-({4-chloro-3-[(3-chloro-5-cyanophenyl)oxy]-2-fluorophenyl}methyl)-1H-pyrrole-2-carboxamide (0.029 g, 8.8% yield) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ ppm 11.87 (br. s., 1H) 7.96 (t, 1H) 7.83 (s, 1H) 7.46-7.54 (m, 3H) 7.40 (t, 1H) 6.96 (t, 1H) 6.25 (t, 1H) 4.56 (d, 2H). MS: m/z 479.9 (M−1).

후처리

  1. customthe layers separated
  2. extractionThe aqueous layer was extracted with EtOAc (3×10 mL)
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customPurification
  7. customFurther purification by RPHPLC
  8. customThe desired fractions were collected
  9. extractionextracted with EtOAc (3×10 mL)
  10. dry with materialdried over sodium sulfate
  11. filtrationfiltered
  12. customevaporated

출처 및 근거

ORD 기록
ord-44c78c1f74324536a8db6abf71a1db41
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304419B2

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