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Triethylamine → HCID 86614670, 화합물

HRID 1433767
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HRID 1433767 반응식
[CH2:1]([O:8][C:9](=[O:26])[CH:10]([C:19]1[CH:24]=[CH:23][C:22](Br)=[CH:21][CH:20]=1)[NH:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:27]([S:29]([CH3:32])(=[O:31])=[O:30])=[CH2:28].C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(N(CC)CC)C>C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:1]([O:8][C:9](=[O:26])[CH:10]([NH:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[C:19]1[CH:24]=[CH:23][C:22](/[CH:28]=[CH:27]/[S:29]([CH3:32])(=[O:31])=[O:30])=[CH:21][CH:20]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 19354Methyl vinyl sulfoneHCID 80271Tri-o-tolylphosphineHCID 68620118HCID 68620118, 화합물

생성물 1

HCID 86614670HCID 86614670, 화합물수율 75%

시약·촉매·용매 2

HCID 167845palladium(II) acetate
촉매
HCID 6342Acetonitrile용매

실험 절차

(4-Bromo-phenyl)-tert-butoxycarbonylamino-acetic acid benzyl ester (1.5 g, 3.6 mmol), methyl vinyl sulfone (406 μL, 4.6 mmol), palladium(II) acetate (80 mg, 10 mol %), tri-o-tolylphosphine (217 mg, 20 mol %) and triethylamine (2.0 ml, 14.3 mmol) were combined in acetonitrile (18 mL), degassed and refluxed for 8 hours. Additional palladium(II) acetate (80 mg, 10 mol %) and tri-o-tolylphosphine (217 mg, 20 mol %) were added and refluxing continued overnight. The reaction was cooled, solvent removed in vacuo and the residue was purified by chromatography over silica gel gradient eluted from 20 to 90% v/v ethyl acetate in hexane to afford tert-butoxycarbonylamino-[4-((E)-2-methanesulfonyl-vinyl)-phenyl]-acetic acid benzyl ester (1.2 g, 75%).

후처리

  1. customdegassed
  2. temperaturerefluxed for 8 hours
  3. additionAdditional palladium(II) acetate (80 mg, 10 mol %) and tri-o-tolylphosphine (217 mg, 20 mol %) were added
  4. temperaturerefluxing continued overnight
  5. temperatureThe reaction was cooled
  6. customsolvent removed in vacuo
  7. customthe residue was purified by chromatography over silica gel gradient
  8. washeluted from 20 to 90% v/v ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-58261898644d4049b6b31fbc4b0c4f31
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612212B2

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