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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 86680886, 화합물 → HCID 52945927, 화합물

HRID 1914861
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HRID 1914861 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([NH:12][C:13]2[CH:18]=[C:17]([N+:19]([O-:21])=[O:20])[CH:16]=[CH:15][C:14]=2[OH:22])=S)=[CH:5][CH:4]=1)[CH3:2]>C(#N)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]2[O:22][C:14]3[CH:15]=[CH:16][C:17]([N+:19]([O-:21])=[O:20])=[CH:18][C:13]=3[N:12]=2)=[CH:5][CH:4]=1)[CH3:2]
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참가 물질

3

반응물 1

HCID 86680886HCID 86680886, 화합물

생성물 1

HCID 52945927HCID 52945927, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

In an ice bath under nitrogen gas, 15 mL of acetonitrile was slowly added to KO2 (12.05 mmol, 5 eq) with stirring. Then, the compound (a) synthesized in Example 1 (2.41 mmol, 1 eq) in 20 mL of acetonitrile was slowly added to said solution containing KO2. The mixture was reacted at room temperature for 16 hours, and then the reaction solution was diluted with 30 mL of ice water. This solution was extracted with dichloromethane, and washed two times with saturated aqueous NaCl solution. After drying with anhydrous MgSO4, the precipitate obtained by removing the solvent under reduced pressure was filtered under reduced pressure with EtOAc:hexane=1:10 (V/V) to yield the title compound (b). Yellow powder (88%), mp 172-173° C.; 1H NMR (Acetone-d6, 400 MHz) δ 9.805 (s, 1H), 8.229 (s, 1H), 8.109 (d, J=8.8 Hz, 1H), 7.764 (d, J=8.4 Hz, 2H), 7.615 (d, J=9.2 Hz, 1H), 7.278 (d, J=8.8 Hz, 2H), 2.651 (q, J=7.6 Hz, 2H), 1.230 (t, J=7.6 Hz, 3H).

후처리

  1. additioncontaining KO2
  2. customThe mixture was reacted at room temperature for 16 hours
  3. extractionThis solution was extracted with dichloromethane
  4. washwashed two times with saturated aqueous NaCl solution
  5. dry with materialAfter drying with anhydrous MgSO4
  6. customthe precipitate obtained
  7. customby removing the solvent under reduced pressure
  8. filtrationwas filtered under reduced pressure with EtOAc

출처 및 근거

ORD 기록
ord-711a3274d2584d4f89c476d1e2828c25
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08614240B2

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