Ammonia → HCID 89876230, 화합물

HRID 594102

반응식

HRID 594102 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 89876230HCID 89876230, 화합물수율 69.9%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-b44f110019724f3fb620e6ff3114cbd1
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242972B2

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