Hydroxylamine → HCID 178455217, 화합물

HRID 705350노트

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HRID 705350 반응식
[Si:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]([C:18]1[C:35]([CH:36]2[CH2:38][CH2:37]2)=[CH:34][C:21]2[C:22]([C:32]#[N:33])=[C:23]([C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=3)[O:24][C:20]=2[CH:19]=1)[S:14]([CH3:17])(=[O:16])=[O:15])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[NH2:39][OH:40]>C(O)C>[Si:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]([S:14]([CH3:17])(=[O:16])=[O:15])[C:18]1[C:35]([CH:36]2[CH2:38][CH2:37]2)=[CH:34][C:21]2[C:22]([C:32](=[NH:33])[NH:39][OH:40])=[C:23]([C:25]3[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=3)[O:24][C:20]=2[CH:19]=1)([C:4]([CH3:7])([CH3:5])[CH3:6])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 89955073N-(4-{[tert-butyl(dimethyl)silyl]oxy}butyl)-N-[3-cyano-5-cyclopropyl-2-(4-fluorophenyl)-1-benzo furan-6-yl]methanesulfonamide

생성물 1

HCID 178455217HCID 178455217, 화합물수율 84%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
140 °C

실험 절차

To a 20-mL microwave tube was added a solution of Example 11B (0.1346 g, 0.242 mmol) in ethanol (3 mL) followed by hydroxylamine (50 weight % in water, 3 mL, 50.9 mmol). The tube was sealed and the thick slurry was heated in a microwave reactor (Personal Chemistry (Biotage), Emrys Creator, 300 W maximum) for 30 minutes at 140° C. The reaction mixture was concentrated in vacuo to a cloudy solution that was taken up in ethyl acetate (60 mL), washed with 10% aqueous NaCl, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to afford the title compound as a foamy white solid (0.119 g, 84%).

후처리

  1. customThe tube was sealed
  2. concentrationThe reaction mixture was concentrated in vacuo to a cloudy solution that
  3. washwashed with 10% aqueous NaCl
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-1518a5620e35426ba4488c093397918c
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09173887B2

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