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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 69018939, 화합물 → HCID 69018966, 화합물

HRID 1865113
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HRID 1865113 반응식
[C:1]([C:3]1[C:4]([C:18]2[CH:23]=[CH:22][C:21]([O:24]CC3C=CC=CC=3)=[CH:20][CH:19]=2)=[C:5]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:6]([CH3:12])[C:7]=1[C:8]([F:11])([F:10])[F:9])#[N:2].[H][H]>[OH-].[OH-].[Pd+2].C(O)C.C1COCC1>[C:1]([C:3]1[C:4]([C:18]2[CH:19]=[CH:20][C:21]([OH:24])=[CH:22][CH:23]=2)=[C:5]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:6]([CH3:12])[C:7]=1[C:8]([F:11])([F:9])[F:10])#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 69018939HCID 69018939, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 69018966HCID 69018966, 화합물

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

In a manner analogous to the procedure set forth in Scheme II, step A, hydrogenate ethyl 4-cyano-1-methyl-3-[4-(phenylmethoxy)phenyl]-5-(trifluoromethyl)pyrrole-2-carboxylate, (intermediate prepared in example A-237) using Pearlman's catalyst and 60 psi of hydrogen gas in 1:1 ethanol/THF for 11 hours. Filter the reaction through diatomaceous earth and concentrate in vacuo. Purify the residue via radial chromatography eluting with ethyl acetate and hexane to provide the title compound. MS (m/e): 337.0 (M−1) 1H NMR: 7.20 (d, 2H, J=8.3 Hz), 6.84 (d, 2H, J=8.8 Hz), 5.85 (s, 1H), 4.16 (q, 2H, J=7.0 Hz), 4.05 (s, 3H), 1.07 (t, 3H, J=7.0 Hz)

후처리

  1. customfor 11 hours
  2. filtrationFilter
  3. customthe reaction through diatomaceous earth
  4. concentrationconcentrate in vacuo
  5. customPurify the residue via radial chromatography
  6. washeluting with ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-351827c889d54699b5e9cbd1f7253837
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07625932B2

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