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Sodium Carbonate → HCID 68705441, 화합물

HRID 1988858
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HRID 1988858 반응식
Cl.[CH2:2]([N:9]1[C:17]2[C:12](=[N:13][CH:14]=[C:15]([Br:27])[C:16]=2[O:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=2)[C:11]([CH3:28])=[C:10]1[CH3:29])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(=O)([O-])[O-].[Na+].[Na+]>>[CH2:2]([N:9]1[C:17]2[C:12](=[N:13][CH:14]=[C:15]([Br:27])[C:16]=2[O:18][CH2:19][C:20]2[CH:21]=[CH:22][C:23]([F:26])=[CH:24][CH:25]=2)[C:11]([CH3:28])=[C:10]1[CH3:29])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
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참가 물질

3

반응물 2

HCID 10340Sodium CarbonateHCID 68705958HCID 68705958, 화합물

생성물 1

HCID 68705441HCID 68705441, 화합물

실험 절차

1-Benzyl-6-bromo-7-(4-fluorobenzyloxy)-2,3-dimethyl-1H-pyrrolo[3,2-b]pyridine hydrochloride prepared in Example 273 was neutralized with a saturated sodium carbonate solution to obtain 1-benzyl-6-bromo-7-(4-fluoro-benzyloxy)-2,3-dimethyl-1H-pyrrolo[3,2-b]pyridine (1.4 g, 3.18 mmol). A solution of 1-benzyl-6-bromo-7-(4-fluoro-benzyloxy)-2,3-dimethyl-1H-pyrrolo[3,2-b]pyridine (1.4 g, 3.18 mmol) and copper (I) cyanide (700 mg, 7.52 mmol) in anhydrous N,N-dimethylformamide (30 ml) was refluxed for 48 hours and then cooled to room temperature. Ethyl acetate was added to the reaction mixture, which was then filtered to discard insoluble solid. Water was added to the resulting solution, which was then extracted with ethyl acetate. The resulting organic layer was dried on anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified with silica gel column chromatography (ethyl acetate/methanol=10/1, v/v) to give 278 mg of the titled compound as a white solid.

출처 및 근거

ORD 기록
ord-e970035d45df4873a533fb0f7be90f47
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07642269B2

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