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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 58370136, 화합물 → HCID 68840871, 화합물

HRID 1889281
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HRID 1889281 반응식
[CH3:1][O:2][C:3](=[O:21])[C:4]([NH:7][C:8]([C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]=1Br)=[O:9])([CH3:6])[CH3:5]>C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[CH3:1][O:2][C:3](=[O:21])[C:4]([CH3:6])([NH:7][C:8]([C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]=1[C:16]#[C:15][CH2:14][CH2:13][C:12]1[CH:17]=[CH:18][CH:19]=[CH:10][CH:11]=1)=[O:9])[CH3:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 58370136HCID 58370136, 화합물

생성물 1

HCID 68840871HCID 68840871, 화합물수율 109.6%

시약·촉매·용매 1

HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매

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온도
130 °C

실험 절차

40 mg 2-[(1-bromo-naphthalene-2-carbonyl)-amino]-2-methyl-propionic acid methyl ester and 0.8 mg bis(triphenylphosphine)palladium(II)chloride were placed in a reaction vial, which was evaporated and backfilled with argon three times. Via septum 18 mg of 4-phenyl-1-butyne, 180 μl diethylamine and 0.2 ml abs. DMF were added. In a microwave reactor the reaction was heated to 130° C. for 5 min. Then, water and ethyl acetate were added, the layers were separated, and the aqueous phase was extracted with ethyl acetate twice. The combined organic layers were dried over magnesium sulphate and concentrated. The resulting residue was purified by chromatography on silica (ethyl acetate/heptane) to yield 25 mg of 2-methyl-2-{[1-(4-phenyl-but-1-ynyl)-naphthalene-2-carbonyl]-amino}-propionic acid methyl ester.

후처리

  1. customwhich was evaporated
  2. additionDMF were added
  3. additionThen, water and ethyl acetate were added
  4. customthe layers were separated
  5. extractionthe aqueous phase was extracted with ethyl acetate twice
  6. dry with materialThe combined organic layers were dried over magnesium sulphate
  7. concentrationconcentrated
  8. customThe resulting residue was purified by chromatography on silica (ethyl acetate/heptane)

출처 및 근거

ORD 기록
ord-1a961a147c86461ab56027082f8a4416
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08501981B2

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