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Diisopropylethylamine → HCID 117856350, 화합물

HRID 509915
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HRID 509915 반응식
[NH2:1][C:2]1[C:3]([C:10]([OH:12])=O)=[N:4][C:5]([Cl:9])=[C:6]([NH2:8])[N:7]=1.FC(F)(F)C([O-])=O.[Br-].[NH2:21][CH:22]1[CH2:27][CH2:26][CH2:25][N+:24]([CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])([CH2:28][CH2:29][CH2:30][C:31]2[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[CH:33][CH:32]=2)[CH2:23]1.NC1CCC[N+](CCCC2C=CC(OC)=CC=2)(CC(OCC)=O)C1.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.C(N(CC)C(C)C)(C)C>CN(C)C=O>[Cl-:9].[NH2:1][C:2]1[C:3]([C:10]([NH:21][CH:22]2[CH2:27][CH2:26][CH2:25][N+:24]([CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])([CH2:28][CH2:29][CH2:30][C:31]3[CH:32]=[CH:33][C:34]([O:37][CH3:38])=[CH:35][CH:36]=3)[CH2:23]2)=[O:12])=[N:4][C:5]([Cl:9])=[C:6]([NH2:8])[N:7]=1
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참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 64521193,5-Diamino-6-chloro-pyrazine acid2회HCID 131733252HCID 131733252, 화합물2회

생성물 1

HCID 117856350HCID 117856350, 화합물

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

A solution of 3,5-diamino-6-chloropyrazine-2-carboxylic-acid (Intermediate 1.1.1, 46 mg, 0.25 mmol), 3-amino-1-ethoxycarbonylmethyl-1-[3-(4-methoxy-phenyl)-propyl]-piperidinium bromide trifluoroacetate salt (Intermediate 3.1.2, 230 mg, 0.25 mmol), O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (86 mg, 0.27 mmol) and N,N-diisopropylethylamine (0.15 mL, 0.1 mmol) in dry N,N-dimethylformamide (5 mL) is stirred for 5 hours at room temperature. The solution is concentrated under reduced pressure to half of the volume, water (2 mL) added and the mixture purified via preparative reverse phase HPLC (gradient of acetonitrile in water+0.05% trifluoroacetic acid). Fractions containing the title compound are concentrated under reduced pressure. The residue is treated with HCl in diethyl ether (2 M, 2 mL), the solvent removed and the residue dried at 50° C. under vacuum. Yield: 56 mg. IC50=0.15.

후처리

  1. concentrationThe solution is concentrated under reduced pressure to half of the volume, water (2 mL)
  2. additionadded
  3. customthe mixture purified via preparative reverse phase HPLC (gradient of acetonitrile in water+0.05% trifluoroacetic acid)
  4. additionFractions containing the title compound
  5. concentrationare concentrated under reduced pressure
  6. additionThe residue is treated with HCl in diethyl ether (2 M, 2 mL)
  7. customthe solvent removed
  8. customthe residue dried at 50° C. under vacuum

출처 및 근거

ORD 기록
ord-a3a5e5c9a2dd48328160d8f249c6d336
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096548B2

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