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1,2-Dichloroethane → HCID 178521725, compound

HRID 1047555
Notes
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Reaction equation

HRID 1047555 reaction equation
[F:1][C:2]1([F:8])[CH2:4][CH:3]1[C:5](O)=[O:6].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.C(=O)(O)[O-].[Na+].[O:28]1[CH2:33][CH2:32][N:31]([CH2:34][C:35]2[CH:36]=[CH:37][C:38]3[N:42]=[C:41]([C:43]4[C:51]5[C:46](=[CH:47][CH:48]=[C:49]([NH2:52])[CH:50]=5)[N:45]([CH:53]5[CH2:58][CH2:57][CH2:56][CH2:55][O:54]5)[N:44]=4)[NH:40][C:39]=3[CH:59]=2)[CH2:30][CH2:29]1>CN(C=O)C>[F:1][C:2]1([F:8])[CH2:4][CH:3]1[C:5]([NH:52][C:49]1[CH:50]=[C:51]2[C:46](=[CH:47][CH:48]=1)[N:45]([CH:53]1[CH2:58][CH2:57][CH2:56][CH2:55][O:54]1)[N:44]=[C:43]2[C:41]1[NH:42][C:38]2[CH:37]=[CH:36][C:35]([CH2:34][N:31]3[CH2:32][CH2:33][O:28][CH2:29][CH2:30]3)=[CH:59][C:39]=2[N:40]=1)=[O:6]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 27828232,2-Difluorocyclopropane-1-carboxylic acidHCID 1363522593-(6-(morpholinomethyl)-1H-benzo[d]imidazol-2-yl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-amine

Product 1

HCID 178521725
HCID 178521725, compound
Yield 81%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

2,2-Difluorocyclopropane carboxylic acid (3 mg, 0.024 mmol), HOBt (5 mg, 0.037 mmol), EDC (6.6 mg, 0.035 mmol) and sodium bicarbonate (2 mg, 0.024 mmol) were added to a solution of 3-(6-(morpholinomethyl)-1H-benzo[d]imidazol-2-yl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-amine (10 mg, 0.023 mmol) in DMF (5 mL). The reaction mixture was stirred at room temperature for 24 h, and then the solvent was removed in vacuo. Purification by flash chromatography (6% CH3OH/CH2Cl2) yielded the title compound (10 mg) as a solid. 1H NMR: (400 MHz, CD3OD): δ 8.62 (s, 1H), 7.75-7.66 (m, 4H), 7.34 (d, 1H, J=8.0 Hz), 5.94 (dd, 1H, J=2.8 and 9.6 Hz), 4.01 (m, 3H), 3.85 (m, 1H), 3.77 (m, 4H), 2.81 (m, 4H), 2.68 (m, 1H), 2.18-2.10 (m, 3H), 1.91-1.83 (m, 3H), 1.71 (m, 2H); ESI-MS [M+H]+: 537.2.

Workup

  1. customthe solvent was removed in vacuo
  2. customPurification by flash chromatography (6% CH3OH/CH2Cl2)

Sources & evidence

ORD record
ord-2f9e6299d09b4f4b910cfe2e145577e9
Source dataset
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08569511B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes