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Potassium Carbonate → HCID 89761783, 화합물

HRID 528573
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HRID 528573 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]([CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)[C:12]2[S:13][CH:14]=[CH:15][N:16]=2)(=[O:10])=[O:9])=[CH:4][C:3]=1[OH:26].C([O-])([O-])=O.[K+].[K+].Cl[CH:34]([CH3:38])[C:35](Cl)=[O:36]>CN(C=O)C>[CH3:25][O:24][C:21]1[CH:22]=[CH:23][C:18]([CH2:17][N:11]([C:12]2[S:13][CH:14]=[CH:15][N:16]=2)[S:8]([C:5]2[CH:6]=[CH:7][C:2]3[NH:1][C:35](=[O:36])[CH:34]([CH3:38])[O:26][C:3]=3[CH:4]=2)(=[O:9])=[O:10])=[CH:19][CH:20]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1110192-Chloropropionyl chlorideHCID 89761412HCID 89761412, 화합물

생성물 1

HCID 89761783HCID 89761783, 화합물수율 63.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
25 °C

실험 절차

To a solution of 4-amino-3-hydroxy-N-(4-methoxybenzyl)-N-(thiazol-2-yl)benzenesulfonamide (INTERMEDIATE AD) (2.0 g, 5.12 mmol) in DMF (15 mL) was added K2CO3 (2.1 g, 15.3 mmol, Quaigens). To the above suspension was added 2-chloropropanoyl chloride (0.780 g, 6.15 mmol) at 0° C. and reaction mixture was stirred at 25° C. for 30 min, then heated 60° C. for 3 h. The reaction mixture was cooled to 25° C. The organic compound was extracted with EtOAc, washed with water, dried over sodium sulfate and concentrated. The resulting residue was purified by silica gel column chromatography using a gradient of 0-50% EtOAc in hexanes as the eluent to afford 1.45 g of N-(4-methoxybenzyl)-2-methyl-3-oxo-N-(thiazol-2-yl)-3,4-dihydro-2H-benzo[b][1,4]oxazine-7-sulfonamide as off white solid in 63.6% yield. 1H-NMR (400 MHz, DMSO): δ 7.45-7.46 (m, 2H), 7.40-7.44 (m, 1H), 7.23-7.26 (m, 3H), 7.02 (d, J=8.4 Hz, 1H), 6.85 (d, J=8.8 Hz, 2H), 5.19 (s, 2H), 3.70 (s, 3H), 1.44 (t, J=6.8 Hz, 3H); m/z (ESI, positive ion) 445.9 (M+H).

후처리

  1. customreaction mixture
  2. temperatureheated 60° C. for 3 h
  3. temperatureThe reaction mixture was cooled to 25° C
  4. extractionThe organic compound was extracted with EtOAc
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated
  8. customThe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-e21bf3adbe964b998baa604413c57e09
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346798B2

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