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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 25256072, 화합물 → HCID 25256481, 화합물

HRID 1950853
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인쇄 미리보기

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HRID 1950853 반응식
[F:1][C:2]1([F:33])[CH2:7][CH2:6][CH2:5][N:4]([C:8]2[CH:13]=[CH:12][C:11]([C:14]3[O:18][N:17]=[C:16]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=4[O:25][C:26]([F:29])([F:28])[F:27])[N:15]=3)=[CH:10][C:9]=2[N+:30]([O-])=O)[CH2:3]1>CCO.C([O-])(O)=O.[Na+]>[F:33][C:2]1([F:1])[CH2:7][CH2:6][CH2:5][N:4]([C:8]2[CH:13]=[CH:12][C:11]([C:14]3[O:18][N:17]=[C:16]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=4[O:25][C:26]([F:27])([F:28])[F:29])[N:15]=3)=[CH:10][C:9]=2[NH2:30])[CH2:3]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 25256072HCID 25256072, 화합물

생성물 1

HCID 25256481HCID 25256481, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 516892Sodium Bicarbonate용매

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온도
70 °C

실험 절차

Stannous chloride dihydrate (478 mg; 2.13 mmol; 5 eq.) was added to a solution of Example 11 (200 mg; 0.43 mmol; 1 eq.) in EtOH (20 mL) and the resulting mixture was stirred at 70° C. for 3 hours, then at room temperature for 16 hours. The solution was diluted with sat. aq. NaHCO3 and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuo. Purification by column chromatography (c-hexane/ethyl acetate, 70/30) followed by crystallization from n-pentane afforded the title compound as an off-white solid.

후처리

  1. waitat room temperature for 16 hours
  2. extractionextracted with ethyl acetate
  3. washThe combined organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customPurification by column chromatography (c-hexane/ethyl acetate, 70/30)
  7. customfollowed by crystallization from n-pentane

출처 및 근거

ORD 기록
ord-28452c7c2f574b4781684c20f9e86720
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404676B2

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