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2-Naphthoic acid → HCID 59514514, 화합물

HRID 2422146
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HRID 2422146 반응식
[CH3:1][O:2][C:3](=[O:21])[CH2:4][C:5]1[C:6]([Cl:20])=[N:7][C:8]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=2)=[N:9][C:10]=1[Cl:11].[CH:22]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:25]=[CH:24][C:23]=1[C:32](O)=[O:33].CCOC(C)=O>C1COCC1>[Cl:20][C:6]1[C:5]([CH2:4][C:3]([O:2][CH3:1])=[O:21])=[C:10]([Cl:11])[N:9]=[C:8]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([NH:19][C:32]([C:23]3[CH:24]=[CH:25][C:26]4[C:31](=[CH:30][CH:29]=[CH:28][CH:27]=4)[CH:22]=3)=[O:33])=[CH:15][CH:14]=2)[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 71232-Naphthoic acidHCID 8857Ethyl AcetateHCID 59514483HCID 59514483, 화합물

생성물 1

HCID 59514514HCID 59514514, 화합물수율 669.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of methyl[2-(4-aminobenzyl)-4,6-dichloropyrimidin-5-yl]acetate (0.073 g, 0.23 mmol), 2-naphthoic acid (0.048 g, 0.028 mmol), and WSCI (0.049 g, 0.026 mmol) in anhydrous THF (3 mL) was stirred at room temperature under Ar atmosphere for 10 hours. EtOAc (80 mL) was then introduced and the organic phase was washed sequentially with saturated NaHCO3, water, and brine, dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The crude product thus obtained as a light orange oil was triturated with diisopropyl ether and the separated solids was collected by suction to give methyl {4,6-dichloro-2-[4-(2-naphthoylamino)benzyl]pyrimidin-5-yl}acetate (0.090 g, 78% yield) as a white powder.

후처리

  1. washthe organic phase was washed sequentially with saturated NaHCO3, water, and brine
  2. dry with materialdried over anhydrous MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe crude product thus obtained as a light orange oil
  6. customwas triturated with diisopropyl ether
  7. customthe separated solids was collected by suction

출처 및 근거

ORD 기록
ord-cdf5425743fb469e8b9efc5059093b75
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960393B2

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