Ammonia → HCID 89876230、化合物

HRID 594102

反応式

HRID 594102 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](Cl)(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:19])[O:4][N:3]=1.[NH3:20]>CO>[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([NH2:20])(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:19])[O:4][N:3]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 164907024-((3,5-Dimethylisoxazol-4-yl)methoxy)benzene-1-sulfonyl chloride

生成物 1

HCID 89876230HCID 89876230、化合物収率 69.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
20 °C

実験手順

4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}benzenesulfonyl chloride (300 mg, 0.994 mmol) was added to ammonia solution (2 mL, 92 mmol, 0.88 NH3 in water). The reaction was stirred at 20° C. for 30 minutes, then left to stand overnight. The reaction mixture was diluted with methanol (5 mL) and passed sequentially through two separate aminopropyl (NH2) solid phase extraction (SPE) cartridges eluting with methanol. The product-containing fractions were combined and evaporated in vacuo to give product as a yellow solid (196.2 mg). LCMS (2 min, formic) Rt 0.71 min, m/z (ES+) 283 (M+H).

後処理

  1. waitleft
  2. waitto stand overnight
  3. customseparate
  4. extractionaminopropyl (NH2) solid phase extraction (SPE) cartridges
  5. washeluting with methanol
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-b44f110019724f3fb620e6ff3114cbd1
出典データセット
uspto-grants-2016_01
特許番号
US09242972B2

関連ノート

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