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Chlorosulfamic acid → HCID 86730127, 화합물

HRID 1467362
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HRID 1467362 반응식
[NH2:1][C:2]1[C:3]([C:22]#[N:23])=[C:4]([CH:19]=[CH:20][CH:21]=1)[O:5][CH2:6][C:7]([NH:10][C:11](=[O:18])[C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1)([CH3:9])[CH3:8].[S:24](Cl)(=[O:27])(=[O:26])[NH2:25].C([O-])(O)=O.[Na+]>CC(N(C)C)=O>[C:22]([C:3]1[C:2]([NH:1][S:24](=[O:27])(=[O:26])[NH2:25])=[CH:21][CH:20]=[CH:19][C:4]=1[O:5][CH2:6][C:7]([NH:10][C:11](=[O:18])[C:12]1[CH:13]=[CH:14][N:15]=[CH:16][CH:17]=1)([CH3:9])[CH3:8])#[N:23]
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참가 물질

5

반응물 3

HCID 24499Chlorosulfamic acidHCID 516892Sodium BicarbonateHCID 867301281622458-78-9

생성물 1

HCID 86730127HCID 86730127, 화합물수율 90.4%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

To a solution of N-(1-(3-amino-2-cyanophenoxy)-2-methylpropan-2-yl)isonicotinamide (10.76 g, 34.67 mmol) in DMA (35 mL) was added sulfamoyl chloride (7.98 g, 69.34 mmol) at room temperature under nitrogen. The reaction mixture was then stirred at room temperature under nitrogen overnight. The resulting solution was poured into 200 mL of ice cooled NaHCO3 aqueous and stirred for 30 minutes, the precipitate was collected by filtration, after dry obtained 12.2 g of clean product as an off white solid in 90% yield. 1H NMR (400 MHz, DMSO-d6) δ 1.47 (s, 6H), 4.32 (s, 2H), 6.93 (d, J=8.8 Hz, 1H), 7.12 (d, J=8.0 Hz, 1H), 7.23 (s, 2H), 7.53 (t, J=8.8 Hz, 1H), 7.67 (d, J=6 Hz, 2H), 8.29 (s, 1H), 8.66 (d, J=6.4 Hz, 2H), 9.45 (s, 1H). MS 390 (MH+).

후처리

  1. stirringstirred for 30 minutes
  2. filtrationthe precipitate was collected by filtration
  3. customafter dry

출처 및 근거

ORD 기록
ord-79d60cf5802b4193b8fe999a5f13d503
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09000151B2

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