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Morpholine → HCID 67147485, 화합물

HRID 490430
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HRID 490430 반응식
F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[CH3:25][O:26][C:27]1[CH:28]=[C:29]2[C:33](=[CH:34][C:35]=1[O:36][CH3:37])[N:32]([CH2:38][CH2:39][C:40]([OH:42])=O)[CH:31]=[C:30]2[C:43]1[NH:51][C:46]2=[N:47][CH:48]=[CH:49][CH:50]=[C:45]2[CH:44]=1.[NH:52]1[CH2:57][CH2:56][O:55][CH2:54][CH2:53]1.C(N(C(C)C)CC)(C)C>CN(C)C=O.C(OCC)(=O)C.O>[CH3:25][O:26][C:27]1[CH:28]=[C:29]2[C:33](=[CH:34][C:35]=1[O:36][CH3:37])[N:32]([CH2:38][CH2:39][C:40]([N:52]1[CH2:57][CH2:56][O:55][CH2:54][CH2:53]1)=[O:42])[CH:31]=[C:30]2[C:43]1[NH:51][C:46]2=[N:47][CH:48]=[CH:49][CH:50]=[C:45]2[CH:44]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 67147433HCID 67147433, 화합물

생성물 1

HCID 67147485HCID 67147485, 화합물

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

실험 절차

0.036 g of O-(1H-benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate is added to a solution of 0.035 g of 3-[5,6-dimethoxy-3-(1H-pyrrolo[2,3-b]pyridin-2-yl)indol-1-yl]propionic acid in 3 ml of dimethylformamide, under an inert argon atmosphere at a temperature in the region of 20° C. The reaction medium is agitated at this temperature for 1 hour. 0.01 ml of morpholine and then 0.017 ml of diisopropylethylamine are added. After agitation at the same temperature for 3 hours, 10 ml of water and 10 ml of ethyl acetate are added. After separation by settling out, the organic phase is dried over sodium sulfate, filtered, and then concentrated under reduced pressure. The residue obtained is purified by flash-pack chromatography (silica, 98/02 by volume dichloromethane/methanol as eluents). The fractions containing the product are concentrated under reduced pressure. 0.025 g of 3-[5,6-dimethoxy-3-(1H-pyrrolo[2,3-b]pyridin-2-yl)indol-1-yl]-1-morpholin-4-ylpropan-1-one is thus obtained, the characteristics of which are as follows:

후처리

  1. waitAfter agitation at the same temperature for 3 hours
  2. customAfter separation
  3. dry with materialthe organic phase is dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue obtained
  7. customis purified by flash-pack chromatography (silica, 98/02 by volume dichloromethane/methanol as eluents)
  8. additionThe fractions containing the product
  9. concentrationare concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-af6381b9e4984ffeac980d1251c54130
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528147B2

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