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1-Bromo-2-methylpropane → 4-((3,5-dimethylisoxazol-4-yl)-methoxy)-N-isobutyl-N-(6-methoxypyridazin-3-yl)benzenesulfonamide

HRID 594153
ノート
印刷プレビュー

反応式

HRID 594153 の反応式
[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([NH:18][C:19]3[N:20]=[N:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=3)(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:27])[O:4][N:3]=1.[CH3:28][C:29](N=C(N(C)C)N(C)C)([CH3:31])[CH3:30].BrCC(C)C>C(#N)C.CO>[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([N:18]([CH2:28][CH:29]([CH3:31])[CH3:30])[C:19]3[N:20]=[N:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=3)(=[O:17])=[O:16])=[CH:13][CH:14]=2)=[C:5]([CH3:27])[O:4][N:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 65551-Bromo-2-methylpropaneHCID 35715812-tert-Butyl-1,1,3,3-tetramethylguanidineHCID 1179259484-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}-N-[6-(methyloxy)-3-pyridazinyl]benzenesulfonamide

生成物 1

HCID 721942794-((3,5-dimethylisoxazol-4-yl)-methoxy)-N-isobutyl-N-(6-methoxypyridazin-3-yl)benzenesulfonamide収率 5.5%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 6342Acetonitrile溶媒

反応条件

温度
20 °C

実験手順

To a solution of 4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}-N-[6-(methyloxy)-3-pyridazinyl]benzenesulfonamide (16 mg, 0.041 mmol) in acetonitrile (1 mL) stirred at room temperature was added N″-(1,1-dimethylethyl)-N,N,N′,N′-tetramethylguanidine (7.02 mg, 0.041 mmol). The reaction mixture was stirred at 20° C. for 1 hour, then 1-bromo-2-methylpropane (8.91 μL, 0.082 mmol) was added. The reaction was heated by microwaves to 150° C. for 15 minutes. After cooling, the reaction mixture was diluted with methanol and passed through an aminopropyl (NH2) solid phase extraction (SPE) cartridge followed by a sulphonic acid (SCX) SPE cartridge, eluting with methanol. The appropriate fractions were combined and evaporated under a stream of nitrogen to give the crude product. The crude was purified by mass directed autoprep (formic acid modifier), to provide the title compound (1.0 mg). LCMS (2 min, formic) Rt 1.27 min, m/z (ES+) 447 (M+H).

後処理

  1. temperatureThe reaction was heated by microwaves to 150° C. for 15 minutes
  2. temperatureAfter cooling
  3. extractionpassed through an aminopropyl (NH2) solid phase extraction (SPE) cartridge
  4. washeluting with methanol
  5. customevaporated under a stream of nitrogen
  6. customto give the crude product
  7. customThe crude was purified by mass

出典と根拠

ORDレコード
ord-25bae4f152ea428daa2e54b793570bd5
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242972B2

反応ノート

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