Triethylamine → HCID 23533346, 화합물

HRID 1181974노트

반응식

HRID 1181974 반응식
CN1CCN(C2C=C[C:11]3[C:12](C=2)=[CH:13][CH:14]=[C:15]2[C:20]=3[O:19][C:18]([C:21]([NH:23][C:24]3[CH:29]=[CH:28][C:27]([N:30]4[CH2:35][CH2:34][O:33][CH2:32][CH2:31]4)=[CH:26][CH:25]=3)=[O:22])=[CH:17][C:16]2=[O:36])CC1.C1C=CC2N(O)N=NC=2C=1.CN([C:51]([O:55]N1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.[CH2:70]([N:72]([CH2:75]C)[CH2:73][CH3:74])[CH3:71].COC1C=C([N:85]2CCOCC2)C=CC=1N>CN(C)C1C=CN=CC=1.CN(C)C=O.C(OCC)(=O)C>[CH3:51][O:55][C:29]1[CH:28]=[C:27]([N:30]2[CH2:31][CH2:32][O:33][CH2:34][CH2:35]2)[CH:26]=[CH:25][C:24]=1[NH:23][C:21]([C:18]1[O:19][C:20]2[C:15]([C:16](=[O:36])[CH:17]=1)=[CH:14][CH:13]=[CH:12][C:11]=2[N:85]1[CH2:74][CH2:73][N:72]([CH3:75])[CH2:70][CH2:71]1)=[O:22]

참가 물질

9

반응물 5

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 4149602-Methoxy-4-morpholinoanilineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 69272428HCID 69272428, 화합물

생성물 1

HCID 23533346HCID 23533346, 화합물수율 54%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylic acid hydrochloride (Reference Example 1) (0.10 g, 0.35 mmol), HOBt (0.10 g, 0.7 mmol), TBTU (0.225 g, 0.7 mmol), 4-(dimethylamino) pyridine (0.01 g, catalytic amount), triethylamine (0.15 mL, 1.04 mmol), and commercially available 2-methoxy-4-morpholin-4-yl-phenylamine (SALOR) (0.08 g, 0.38 mmol) were dissolved in dimethylformamide (2.5 mL) and stirred at room temperature overnight. Ethyl acetate (150 mL) was added and the resulting mixture was washed with water (3×50 mL), dried (Na2SO4), filtered, concentrated under vacuum and triturated with ether to yield a yellow solid (85 mg, 54%). LCMS: m/z=480.3.

후처리

  1. washthe resulting mixture was washed with water (3×50 mL)
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum
  5. customtriturated with ether

출처 및 근거

ORD 기록
ord-8f352da88f9d4dc5aaed9dc07b6b8605
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285662B2

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